Preparation of uranium compounds

DOEpatents

Kiplinger, Jaqueline L; Montreal, Marisa J; Thomson, Robert K; Cantat, Thibault; Travia, Nicholas E

2013-02-19

UI.sub.3(1,4-dioxane).sub.1.5 and UI.sub.4(1,4-dioxane).sub.2, were synthesized in high yield by reacting turnings of elemental uranium with iodine dissolved in 1,4-dioxane under mild conditions. These molecular compounds of uranium are thermally stable and excellent precursor materials for synthesizing other molecular compounds of uranium including alkoxide, amide, organometallic, and halide compounds.

High loading uranium fuel plate

DOEpatents

Wiencek, Thomas C.; Domagala, Robert F.; Thresh, Henry R.

1990-01-01

Two embodiments of a high uranium fuel plate are disclosed which contain a meat comprising structured uranium compound confined between a pair of diffusion bonded ductile metal cladding plates uniformly covering the meat, the meat having a uniform high fuel loading comprising a content of uranium compound greater than about 45 Vol. % at a porosity not greater than about 10 Vol. %. In a first embodiment, the meat is a plurality of parallel wires of uranium compound. In a second embodiment, the meat is a dispersion compact containing uranium compound. The fuel plates are fabricated by a hot isostatic pressing process.

Ion Mobility Spectrometer Field Test

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

Smith, Nicholas; McLain, Derek; Steeb, Jennifer

The Morpho Saffran Itemizer 4DX Ion Mobility Spectrometer previously used to detect uranium signatures in FY16 was used at the former New Brunswick Facility, a past uranium facility located on site at Argonne National Laboratory. This facility was chosen in an attempt to detect safeguards relevant signatures and has a history of processing uranium at various enrichments, chemical forms, and purities; various chemicals such as nitric acid, uranium fluorides, phosphates and metals are present at various levels. Several laboratories were sampled for signatures of nuclear activities around the laboratory. All of the surfaces that were surveyed were below background levelsmore » of the radioanalytical instrumentation and determined to be radiologically clean.« less

Characterization of uranium bearing material using x-ray fluorescence and direct gamma-rays measurement techniques

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

Mujaini, M., E-mail: madihah@uniten.edu.my; Chankow, N.; Yusoff, M. Z.

2016-01-22

Uranium ore can be easily detected due to various gamma-ray energies emitted from uranium daughters particularly from {sup 238}U daughters such as {sup 214}Bi, {sup 214}Pb and {sup 226}Ra. After uranium is extracted from uranium ore, only low energy gamma-rays emitted from {sup 235}U may be detected if the detector is placed in close contact to the specimen. In this research, identification and characterization of uranium bearing materials is experimentally investigated using direct measurement of gamma-rays from {sup 235}U in combination with the x-ray fluorescence (XRF) technique. Measurement of gamma-rays can be conducted by using high purity germanium (HPGe) detectormore » or cadmium telluride (CdTe) detector while a {sup 57}Coradioisotope-excited XRF spectrometer using CdTe detector is used for elemental analysis. The proposed technique was tested with various uranium bearing specimens containing natural, depleted and enriched uranium in both metallic and powder forms.« less

Method for producing uranium atomic beam source

DOEpatents

Krikorian, Oscar H.

1976-06-15

A method for producing a beam of neutral uranium atoms is obtained by vaporizing uranium from a compound UM.sub.x heated to produce U vapor from an M boat or from some other suitable refractory container such as a tungsten boat, where M is a metal whose vapor pressure is negligible compared to that of uranium at the vaporization temperature. The compound, for example, may be the uranium-rhenium compound, URe.sub.2. An evaporation rate in excess of about 10 times that of conventional uranium beam sources is produced.

Validation of gamma-ray detection techniques for safeguards monitoring at natural uranium conversion facilities

DOE PAGES

Dewji, Shaheen A.; Lee, Denise L.; Croft, Stephen; ...

2016-03-28

Recent IAEA circulars and policy papers have sought to implement safeguards when any purified aqueous uranium solution or uranium oxides suitable for isotopic enrichment or fuel fabrication exists. Under the revised policy, IAEA Policy Paper 18, the starting point for nuclear material under safeguards was reinterpreted, suggesting that purified uranium compounds should be subject to safeguards procedures no later than the first point in the conversion process. In response to this technical need, a combination of simulation models and experimental measurements were employed to develop and validate concepts of nondestructive assay monitoring systems in a natural uranium conversion plant (NUCP).more » In particular, uranyl nitrate (UO 2(NO 3) 2) solution exiting solvent extraction was identified as a key measurement point (KMP), where gamma-ray spectroscopy was selected as the process monitoring tool. The Uranyl Nitrate Calibration Loop Equipment (UNCLE) facility at Oak Ridge National Laboratory was employed to simulate the full-scale operating conditions of a purified uranium-bearing aqueous stream exiting the solvent extraction process in an NUCP. Nondestructive assay techniques using gamma-ray spectroscopy were evaluated to determine their viability as a technical means for drawing safeguards conclusions at NUCPs, and if the IAEA detection requirements of 1 significant quantity (SQ) can be met in a timely way. This work investigated gamma-ray signatures of uranyl nitrate circulating in the UNCLE facility and evaluated various gamma-ray detector sensitivities to uranyl nitrate. These detector validation activities include assessing detector responses to the uranyl nitrate gamma-ray signatures for spectrometers based on sodium iodide, lanthanum bromide, and high-purity germanium detectors. The results of measurements under static and dynamic operating conditions at concentrations ranging from 10–90 g U/L of natural uranyl nitrate are presented. A range of gamma-ray lines is examined, including attenuation for transmission measurement of density and concentration. It was determined that transmission-corrected gamma-ray spectra provide a reliable way to monitor the 235U concentration of uranyl nitrate solution in transfer pipes in NUCPs. Furthermore, existing predictive and analysis methods are adequate to design and realize practical designs. The 137Cs transmission source employed in this work is viable but not optimal for 235U densitometry determination. Validated simulations assessed the viability of 133Ba and 57Co as alternative densitometry sources. All three gamma-ray detectors are viable for monitoring natural uranium feed; although high-purity germanium is easiest to interpret, it is, however, the least attractive as an installation instrument. Overall, for monitoring throughput in a facility such as UNCLE, emulating the uranium concentration and pump speeds of the Springfields conversion facility in the United Kingdom, an uncertainty of less than 0.17% is required in order to detect the diversion of 1 SQ of uranyl nitrate through changes in uranium concentration over an accountancy period of one year with a detection probability of 50%. As a result, calibrated gamma-ray detection systems are capable of determining the concentration of uranium content in NUCPs, it is only in combination with verifiable operator declarations and supporting data, such as flow rate and enrichment, that safeguards conclusions can be drawn.« less

Pyroprocessing of Fast Flux Test Facility Nuclear Fuel

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

B.R. Westphal; G.L. Fredrickson; G.G. Galbreth

Used nuclear fuel from the Fast Flux Test Facility (FFTF) was recently transferred to the Idaho National Laboratory and processed by pyroprocessing in the Fuel Conditioning Facility. Approximately 213 kg of uranium from sodium-bonded metallic FFTF fuel was processed over a one year period with the equipment previously used for the processing of EBR-II used fuel. The peak burnup of the FFTF fuel ranged from 10 to 15 atom% for the 900+ chopped elements processed. Fifteen low-enriched uranium ingots were cast following the electrorefining and distillation operations to recover approximately 192 kg of uranium. A material balance on the primarymore » fuel constituents, uranium and zirconium, during the FFTF campaign will be presented along with a brief description of operating parameters. Recoverable uranium during the pyroprocessing of FFTF nuclear fuel was greater than 95% while the purity of the final electrorefined uranium products exceeded 99%.« less

Pyroprocessing of fast flux test facility nuclear fuel

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

Westphal, B.R.; Wurth, L.A.; Fredrickson, G.L.

Used nuclear fuel from the Fast Flux Test Facility (FFTF) was recently transferred to the Idaho National Laboratory and processed by pyroprocessing in the Fuel Conditioning Facility. Approximately 213 kg of uranium from sodium-bonded metallic FFTF fuel was processed over a one year period with the equipment previously used for the processing of EBR-II used fuel. The peak burnup of the FFTF fuel ranged from 10 to 15 atom% for the 900+ chopped elements processed. Fifteen low-enriched uranium ingots were cast following the electrorefining and distillation operations to recover approximately 192 kg of uranium. A material balance on the primarymore » fuel constituents, uranium and zirconium, during the FFTF campaign will be presented along with a brief description of operating parameters. Recoverable uranium during the pyroprocessing of FFTF nuclear fuel was greater than 95% while the purity of the final electro-refined uranium products exceeded 99%. (authors)« less

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

PRODUCTION OF PURIFIED URANIUM

DOEpatents

Burris, L. Jr.; Knighton, J.B.; Feder, H.M.

1960-01-26

A pyrometallurgical method for processing nuclear reactor fuel elements containing uranium and fission products and for reducing uranium compound; to metallic uranium is reported. If the material proccssed is essentially metallic uranium, it is dissolved in zinc, the sulution is cooled to crystallize UZn/sub 9/ , and the UZn/sub 9/ is distilled to obtain uranium free of fission products. If the material processed is a uranium compound, the sollvent is an alloy of zinc and magnesium and the remaining steps are the same.

URANIUM LEACHING AND RECOVERY PROCESS

DOEpatents

McClaine, L.A.

1959-08-18

A process is described for recovering uranium from carbonate leach solutions by precipitating uranium as a mixed oxidation state compound. Uranium is recovered by adding a quadrivalent uranium carbon;te solution to the carbonate solution, adjusting the pH to 13 or greater, and precipitating the uranium as a filterable mixed oxidation state compound. In the event vanadium occurs with the uranium, the vanadium is unaffected by the uranium precipitation step and remains in the carbonate solution. The uranium-free solution is electrolyzed in the cathode compartment of a mercury cathode diaphragm cell to reduce and precipitate the vanadium.

Thermogravimetric Control of Intermediate Products in the Metallurgy of Uranium; CONTROL TERMOGRAVIMETRICO DE PRODUCTOS INTERMEDIOS DE LA METALURGIA DEL URANIO

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

Sanchez, L.G.; Cellini, R.F.

1959-01-01

The thermal decomposition of some intermediate compounds in the metallurgy of uranium such as uranium peroxide, ammonium uranate, ammonium uranium pentafluoride, uranium tetrafluoride, and UO/sub 2/, were studied using Chevenard's thermobalance. Some data on the pyrolysis of synthetic mixtures of intermediate compounds which may appear during the industrial processing are given. Thermogravimetric methods of control are suggested for use in uranium metallurgy. (tr-auth)

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

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

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Non-destructive chemical analyses of these compounds is important for process and environmental monitoring and X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride,more » and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. These compounds have unique spectral signatures that can be used to identify unknown samples.« less

Determination of uranium in clinical and environmental samples by FIAS-ICPMS

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

Karpas, Z.; Lorber, A.; Halicz, L.

Uranium may enter the human body through ingestion or inhalation. Ingestion of uranium compounds through the diet, mainly drinking water, is a common occurrence, as these compounds are present in the biosphere. Inhalation of uranium-containing particles is mainly an occupational safety problem, but may also take place in areas where uranium compounds are abundant. The uranium concentration in urine samples may serve as an indication of the total uranium body content. A method based on flow injection and inductively coupled plasma mass spectrometry (FIAS-ICPMS) was found to be most suitable for determination of uranium in clinical samples (urine and serum),more » environmental samples (seawater, wells and carbonate rocks) and in liquids consumed by humans (drinking water and commercial beverages). Some examples of the application of the FIAS-ICPMS method are reviewed and presented here.« less

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.

Defense Technical Information Center Thesaurus

DTIC Science & Technology

2000-10-01

acquisition radar 4 + Indicates existence of further generic levels of the term DTIC Thesaurus Actuators Acridines Actinide series (cont.) Activated sintering...BT Heterocyclic compounds+ Uranium+ BT Sintering Acrilan Actinide series compounds Activated sludge process use Acrylonitrile polymers RT Actinide...Waste treatment+ Protactinium compounds Acronyms Thorium compounds+ Activation use Abbreviations Transuranium compounds+ UF Energizing Uranium compounds

Actinium radioisotope products of enhanced purity

DOEpatents

Meikrantz, David Herbert; Todd, Terry Allen; Tranter, Troy Joseph; Horwitz, E. Philip

2010-06-15

A product includes actinium-225 (.sup.225Ac) and less than about 1 microgram (.mu.g) of iron (Fe) per millicurie (mCi) of actinium-225. The product may have a radioisotopic purity of greater than about 99.99 atomic percent (at %) actinium-225 and daughter isotopes of actinium-225, and may be formed by a method that includes providing a radioisotope mixture solution comprising at least one of uranium-233 (.sup.233U) and thorium-229 (.sup.229Th), extracting the at least one of uranium-233 and thorium-229 into an organic phase, substantially continuously contacting the organic phase with an aqueous phase, substantially continuously extracting actinium-225 into the aqueous phase, and purifying the actinium-225 from the aqueous phase. In some embodiments, the product may include less than about 1 nanogram (ng) of iron per millicurie (mCi) of actinium-225, and may include less than about 1 microgram (.mu.g) each of magnesium (Mg), Chromium (Cr), and manganese (Mn) per millicurie (mCi) of actinium-225.

METHOD OF RECOVERING URANIUM COMPOUNDS

DOEpatents

Poirier, R.H.

1957-10-29

S>The recovery of uranium compounds which have been adsorbed on anion exchange resins is discussed. The uranium and thorium-containing residues from monazite processed by alkali hydroxide are separated from solution, and leached with an alkali metal carbonate solution, whereby the uranium and thorium hydrorides are dissolved. The carbonate solution is then passed over an anion exchange resin causing the uranium to be adsorbed while the thorium remains in solution. The uranium may be recovered by contacting the uranium-holding resin with an aqueous ammonium carbonate solution whereby the uranium values are eluted from the resin and then heating the eluate whereby carbon dioxide and ammonia are given off, the pH value of the solution is lowered, and the uranium is precipitated.

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

NASA Astrophysics Data System (ADS)

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.; Eiden, Gregory C.; Pemmaraju, C. D.; Prendergast, David; Duffin, Andrew M.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Chemical analyses of these compounds are important for process and environmental monitoring. X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride, and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. The effect of hydration state on the sample, a potential complication in interpreting oxygen K-edge spectra, is discussed. These compounds have unique spectral signatures that can be used to identify unknown samples.

Preparation of High Purity, High Molecular-Weight Chitin from Ionic Liquids for Use as an Adsorbate for the Extraction of Uranium from Seawater

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

Rogers, Robin

Ensuring a domestic supply of uranium is a key issue facing the wider implementation of nuclear power. Uranium is mostly mined in Kazakhstan, Australia, and Canada, and there are few high-grade uranium reserves left worldwide. Therefore, one of the most appealing potential sources of uranium is the vast quantity dissolved in the oceans (estimated to be 4.4 billion tons worldwide). There have been research efforts centered on finding a means to extract uranium from seawater for decades, but so far none have resulted in an economically viable product, due in part to the fact that the materials that have beenmore » successfully demonstrated to date are too costly (in terms of money and energy) to produce on the necessary scale. Ionic Liquids (salts which melt below 100{degrees}C) can completely dissolve raw crustacean shells, leading to recovery of a high purity, high molecular weight chitin powder and to fibers and films which can be spun directly from the extract solution suggesting that continuous processing might be feasible. The work proposed here will utilize the unprecedented control this makes possible over the chitin fiber a) to prepare electrospun nanofibers of very high surface area and in specific architectures, b) to modify the fiber surfaces chemically with selective extractant capacity, and c) to demonstrate their utility in the direct extraction and recovery of uranium from seawater. This approach will 1) provide direct extraction of chitin from shellfish waste thus saving energy over the current industrial process for obtaining chitin; 2) allow continuous processing of nanofibers for very high surface area fibers in an economical operation; 3) provide a unique high molecular weight chitin not available from the current industrial process, leading to stronger, more durable fibers; and 4) allow easy chemical modification of the large surface areas of the fibers for appending uranyl selective functionality providing selectivity and ease of stripping. The resulting sorbent should prove economically feasible, as well as providing an overall net energy gain.« less

Gamma-ray spectroscopy measurements and simulations for uranium mining

NASA Astrophysics Data System (ADS)

Marchais, T.; Pérot, B.; Carasco, C.; Allinei, P.-G.; Chaussonnet, P.; Ma, J.-L.; Toubon, H.

2018-01-01

AREVA Mines and the Nuclear Measurement Laboratory of CEA Cadarache are collaborating to improve the sensitivity and precision of uranium concentration evaluation by means of gamma measurements. This paper reports gamma-ray spectra, recorded with a high-purity coaxial germanium detector, on standard cement blocks with increasing uranium content, and the corresponding MCNP simulations. The detailed MCNP model of the detector and experimental setup has been validated by calculation vs. experiment comparisons. An optimization of the detector MCNP model is presented in this paper, as well as a comparison of different nuclear data libraries to explain missing or exceeding peaks in the simulation. Energy shifts observed between the fluorescence X-rays produced by MCNP and atomic data are also investigated. The qualified numerical model will be used in further studies to develop new gamma spectroscopy approaches aiming at reducing acquisition times, especially for ore samples with low uranium content.

Mortality (1968-2008) in a French cohort of uranium enrichment workers potentially exposed to rapidly soluble uranium compounds.

PubMed

Zhivin, Sergey; Guseva Canu, Irina; Samson, Eric; Laurent, Olivier; Grellier, James; Collomb, Philippe; Zablotska, Lydia B; Laurier, Dominique

2016-03-01

Until recently, enrichment of uranium for civil and military purposes in France was carried out by gaseous diffusion using rapidly soluble uranium compounds. We analysed the relationship between exposure to soluble uranium compounds and exposure to external γ-radiation and mortality in a cohort of 4688 French uranium enrichment workers who were employed between 1964 and 2006. Data on individual annual exposure to radiological and non-radiological hazards were collected for workers of the AREVA NC, CEA and Eurodif uranium enrichment plants from job-exposure matrixes and external dosimetry records, differentiating between natural, enriched and depleted uranium. Cause-specific mortality was compared with the French general population via standardised mortality ratios (SMR), and was analysed via Poisson regression using log-linear and linear excess relative risk models. Over the period of follow-up, 131 161 person-years at risk were accrued and 21% of the subjects had died. A strong healthy worker effect was observed: all causes SMR=0.69, 95% CI 0.65 to 0.74. SMR for pleural cancer was significantly increased (2.3, 95% CI 1.06 to 4.4), but was only based on nine cases. Internal uranium and external γ-radiation exposures were not significantly associated with any cause of mortality. This is the first study of French uranium enrichment workers. Although limited in statistical power, further follow-up of this cohort, estimation of internal uranium doses and pooling with similar cohorts should elucidate potential risks associated with exposure to soluble uranium compounds. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/

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

Measurement of the Auger parameter and Wagner plot for uranium compounds

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

Holliday, Kiel S.; Siekhaus, Wigbert; Nelson, Art J.

2013-05-15

In this study, the photoemission from the U 4f{sub 7/2} and 4d{sub 5/2} states and the U N{sub 6}O{sub 45}O{sub 45} and N{sub 67}O{sub 45}V x-ray excited Auger transitions were measured for a range of uranium compounds. The data are presented in Wagner plots and the Auger parameter is calculated to determine the utility of this technique in the analysis of uranium materials. It was demonstrated that the equal core-level shift assumption holds for uranium. It was therefore possible to quantify the relative relaxation energies, and uranium was found to have localized core-hole shielding. The position of compounds within themore » Wagner plot made it possible to infer information on bonding character and local electron density. The relative ionicity of the uranium compounds studied follows the trend UF{sub 4} > UO{sub 3} > U{sub 3}O{sub 8} > U{sub 4}O{sub 9}/U{sub 3}O{sub 7} Almost-Equal-To UO{sub 2} > URu{sub 2}Si{sub 2}.« less

Recovery of tritium from tritiated molecules

DOEpatents

Swansiger, William A.

1987-01-01

A method of recovering tritium from tritiated compounds comprises the steps of heating tritiated water and other co-injected tritiated compounds in a preheater to temperatures of about 600.degree. C. The mixture is injected into a reactor charged with a mixture of uranium and uranium dioxide. The injected mixture undergoes highly exothermic reactions with the uranium causing reaction temperatures to occur in excess of the melting point of uranium, and complete decomposition of the tritiated compounds to remove tritium therefrom. The uranium dioxide functions as an insulating material and heat sink preventing the reactor side walls from attaining reaction temperatures to thereby minimize tritium permeation rates. The uranium dioxide also functions as a diluent to allow for volumetric expansion of the uranium as it is converted to uranium dioxide. The reactor vessel is preferably stainless steel of sufficient mass so as to function as a heat sink preventing the reactor side walls from approaching high temperatures. A disposable copper liner extends between the reaction chamber and stainless steel outer vessel to prevent alloying of the uranium with the outer vessel. Apparatus used to carry out the method of the invention is also disclosed.

LIQUID METAL COMPOSITIONS CONTAINING URANIUM

DOEpatents

Teitel, R.J.

1959-04-21

Liquid metal compositions containing a solid uranium compound dispersed therein is described. Uranium combines with tin to form the intermetallic compound USn/sub 3/. It has been found that this compound may be incorporated into a liquid bath containing bismuth and lead-bismuth components, if a relatively small percentage of tin is also included in the bath. The composition has a low thermal neutron cross section which makes it suitable for use in a liquid metal fueled nuclear reactor.

[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.

Decontamination of uranium-contaminated waste oil using supercritical fluid and nitric acid.

PubMed

Sung, Jinhyun; Kim, Jungsoo; Lee, Youngbae; Seol, Jeunggun; Ryu, Jaebong; Park, Kwangheon

2011-07-01

The waste oil used in nuclear fuel processing is contaminated with uranium because of its contact with materials or environments containing uranium. Under current law, waste oil that has been contaminated with uranium is very difficult to dispose of at a radioactive waste disposal site. To dispose of the uranium-contaminated waste oil, the uranium was separated from the contaminated waste oil. Supercritical R-22 is an excellent solvent for extracting clean oil from uranium-contaminated waste oil. The critical temperature of R-22 is 96.15 °C and the critical pressure is 49.9 bar. In this study, a process to remove uranium from the uranium-contaminated waste oil using supercritical R-22 was developed. The waste oil has a small amount of additives containing N, S or P, such as amines, dithiocarbamates and dialkyldithiophosphates. It seems that these organic additives form uranium-combined compounds. For this reason, dissolution of uranium from the uranium-combined compounds using nitric acid was needed. The efficiency of the removal of uranium from the uranium-contaminated waste oil using supercritical R-22 extraction and nitric acid treatment was determined.

SUMMARY TECHNICAL REPORT FOR THE PERIOD JANUARY 1, 1961-MARCH 31, 1961

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

Burgett, R. ed

1961-05-01

Uranium and TBP Recovery from Waste Solvent. Laboratory and pilot-scale tests were carried out which demonstrated (1) that uranium in waste solvent can be removed by slurrying the solvent with activated charcoal, filtering the slurry, and washing the slurry with water and 3% Na/sub 2/CO/sub 3/ and (2) that TBP can be recovered from the waste solvent by splitting the solvent with HCl and distilling the TBP-rich phase. Improvement of Green Salt Quality. Denitration of ammonium uranyl trinitrate yielded a light, finely divided form of gamma -UO/ sub 3/ with a surface area higher than that of conventional batch potmore » powder; however, its reactivity in reduction and hydrofluorination tests was only moderately higher in comparison. Oxidation-reduction cycles were found to increase the reactivity of UO/sub 2/ toward hydrofluorination. The properties of various UO/sub 2/ samples were determined and correlated with the preparative methods used. Dehydration of Winlo Green Salt. About 27 tons of Winlo green salt was successfully dehydrated to a water content of -0.04% in a hydrofluorination reactor bank in the Green Salt Plant. Recovery of Uranium from MgF/sub 2/ Slag. A process for continuously digesting MgF/sub 2/ slag for uranium recovery was successfully tested on a plant scale. In this process, a water slurry of slag is transferred at a fixed rate and reacted with HCl, and the controlled feed rate reduces the hydrogen concentration. Graphite Liner for Bomb Reduction of Green Salt. An evaluation was made on machined graphite as a replacement for jolt-packed MgF/sub 2/ presently used to line reduction vessels for uranium metal production. Best results were obtained with a onepiece graphite liner fitted inside a steel vessel with an annulus of MgF/sub 2/ between liner and pot. Effects of Feed Material on Ingot Chemical Purity and Yields. The effects of various types of uranium feed stock on the chemical purity and yield of ingots were studied. The following results were obtained: (1) The H content was higher in ingots cast from melts contairing more derby material, (2) the O, N, and C contents of samples from ingot tops were signiicantly lower than those from ingot bottoms, (3) the crude ingot yields were lowest for pigots, briquettes, and heat-shocked grade III derbies, (4) pigots were deleterious to ingot chemical purity, (5) degreased drip crops and dingot extrnsion scrap were deleterious to core-to-good-core yield. Alpha Annealing of Uranium. The effect of a high alpha temperature anneal on the structure and growin index of beta heat treated uranium was evaluated. It was found that longer alpha annealing times gave greater recrystallization and that higher temperatures gave more rapid recrystallization. Delays of up to 6 months between beta heat treatment and alpha anneal did not affect either the recrystallization or the growth index. Billet Drilling. A LeBlond-Carlstedt Rapid Borer was tested as a urarium billet drilling machine and found to give satisfactory results, although some tool breakage occurred. (D.L.C.)« less

Direct measurement of 235U in spent fuel rods with Gamma-ray mirrors

NASA Astrophysics Data System (ADS)

Ruz, J.; Brejnholt, N. F.; Alameda, J. B.; Decker, T. A.; Descalle, M. A.; Fernandez-Perea, M.; Hill, R. M.; Kisner, R. A.; Melin, A. M.; Patton, B. W.; Soufli, R.; Ziock, K.; Pivovaroff, M. J.

2015-03-01

Direct measurement of plutonium and uranium X-rays and gamma-rays is a highly desirable non-destructive analysis method for the use in reprocessing fuel environments. The high background and intense radiation from spent fuel make direct measurements difficult to implement since the relatively low activity of uranium and plutonium is masked by the high activity from fission products. To overcome this problem, we make use of a grazing incidence optic to selectively reflect Kα and Kβ fluorescence of Special Nuclear Materials (SNM) into a high-purity position-sensitive germanium detector and obtain their relative ratios.

Uranium induces oxidative stress in lung epithelial cells

PubMed Central

Periyakaruppan, Adaikkappan; Kumar, Felix; Sarkar, Shubhashish; Sharma, Chidananda S.

2009-01-01

Uranium compounds are widely used in the nuclear fuel cycle, antitank weapons, tank armor, and also as a pigment to color ceramics and glass. Effective management of waste uranium compounds is necessary to prevent exposure to avoid adverse health effects on the population. Health risks associated with uranium exposure includes kidney disease and respiratory disorders. In addition, several published results have shown uranium or depleted uranium causes DNA damage, mutagenicity, cancer and neurological defects. In the current study, uranium toxicity was evaluated in rat lung epithelial cells. The study shows uranium induces significant oxidative stress in rat lung epithelial cells followed by concomitant decrease in the antioxidant potential of the cells. Treatment with uranium to rat lung epithelial cells also decreased cell proliferation after 72 h in culture. The decrease in cell proliferation was attributed to loss of total glutathione and superoxide dismutase in the presence of uranium. Thus the results indicate the ineffectiveness of antioxidant system’s response to the oxidative stress induced by uranium in the cells. PMID:17124605

PREPARATION OF HIGH PURITY UF$sub 4$

DOEpatents

Magner, J.E.; Long, R.S.; Ellis, D.A.; Grinstead, R.R.

1962-04-17

S>A process for preparing very highly pure uranous tetrafluoride from impure uranium laden solvent extraction strip solutions, ion exchange process and resin-inpulp process eluate solutions which are at least 8M in hydrochloric acid is described. The process first comprises treating any of the above-mentioned solutions with a reducing agent to reduce the uranium to the + 4 oxidation state, and then contacting the reduced solution with an extractant phase comprising about 10 to 70% of tri-butyl phosphate in an organic solvent-diluent selected from benzene, ethyl-benzene, chlorobenzene, xylene, kerosene, or the like. The uranium is extracted into the extractant phase and is subsequently precipitated by treating the extractant with an aqueous fluoride solution. The highly pure uranous tetrafluoride precipitate is separated from the phases and recovered for subsequent utilization. (AEC)

Semi-automatic version of the potentiometric titration method for characterization of uranium compounds.

PubMed

Cristiano, Bárbara F G; Delgado, José Ubiratan; da Silva, José Wanderley S; de Barros, Pedro D; de Araújo, Radier M S; Dias, Fábio C; Lopes, Ricardo T

2012-09-01

The potentiometric titration method was used for characterization of uranium compounds to be applied in intercomparison programs. The method is applied with traceability assured using a potassium dichromate primary standard. A semi-automatic version was developed to reduce the analysis time and the operator variation. The standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization and compatible with those obtained by manual techniques. Copyright © 2012 Elsevier Ltd. All rights reserved.

Identification of Uranyl Minerals Using Oxygen K-Edge X Ray Absorption Spectroscopy

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

Ward, Jesse D.; Bowden, Mark E.; Resch, Charles T.

2016-03-01

Uranium analysis is consistently needed throughout the fuel cycle, from mining to fuel fabrication to environmental monitoring. Although most of the world’s uranium is immobilized as pitchblende or uraninite, there exists a plethora of secondary uranium minerals, nearly all of which contain the uranyl cation. Analysis of uranyl compounds can provide clues as to a sample’s facility of origin and chemical history. X-ray absorption spectroscopy is one technique that could enhance our ability to identify uranium minerals. Although there is limited chemical information to be gained from the uranium X-ray absorption edges, recent studies have successfully used ligand NEXAFS tomore » study the physical chemistry of various uranium compounds. This study extends the use of ligand NEXAFS to analyze a suite of uranium minerals. We find that major classes of uranyl compounds (carbonate, oxyhydroxide, silicate, and phosphate) exhibit characteristic lineshapes in the oxygen K-edge absorption spectra. As a result, this work establishes a library of reference spectra that can be used to classify unknown uranyl minerals.« less

PRODUCTION OF URANIUM AND THORIUM COMPOUNDS

DOEpatents

Arden, T.V.; Burstall, F.H.; Linstead, R.P.; Wells, R.A.

1955-12-27

Compounds of Th and U are extracted with an organic solvent in the presence of an adsorbent substance which has greater retentivity for impurities present than for the uranium and/or thorium. The preferred adsorbent material is noted as being cellulose. The uranium and thoriumcontaining substances treated are preferably in the form of dissolved nitrates, and the preferred organic solvent is diethyl ether.

Conversion of depleted uranium hexafluoride to a solid uranium compound

DOEpatents

Rothman, Alan B.; Graczyk, Donald G.; Essling, Alice M.; Horwitz, E. Philip

2001-01-01

A process for converting UF.sub.6 to a solid uranium compound such as UO.sub.2 and CaF. The UF.sub.6 vapor form is contacted with an aqueous solution of NH.sub.4 OH at a pH greater than 7 to precipitate at least some solid uranium values as a solid leaving an aqueous solution containing NH.sub.4 OH and NH.sub.4 F and remaining uranium values. The solid uranium values are separated from the aqueous solution of NH.sub.4 OH and NH.sub.4 F and remaining uranium values which is then diluted with additional water precipitating more uranium values as a solid leaving trace quantities of uranium in a dilute aqueous solution. The dilute aqueous solution is contacted with an ion-exchange resin to remove substantially all the uranium values from the dilute aqueous solution. The dilute solution being contacted with Ca(OH).sub.2 to precipitate CaF.sub.2 leaving dilute NH.sub.4 OH.

Harnessing redox activity for the formation of uranium tris(imido) compounds

NASA Astrophysics Data System (ADS)

Anderson, Nickolas H.; Odoh, Samuel O.; Yao, Yiyi; Williams, Ursula J.; Schaefer, Brian A.; Kiernicki, John J.; Lewis, Andrew J.; Goshert, Mitchell D.; Fanwick, Phillip E.; Schelter, Eric J.; Walensky, Justin R.; Gagliardi, Laura; Bart, Suzanne C.

2014-10-01

Classically, late transition-metal organometallic compounds promote multielectron processes solely through the change in oxidation state of the metal centre. In contrast, uranium typically undergoes single-electron chemistry. However, using redox-active ligands can engage multielectron reactivity at this metal in analogy to transition metals. Here we show that a redox-flexible pyridine(diimine) ligand can stabilize a series of highly reduced uranium coordination complexes by storing one, two or three electrons in the ligand. These species reduce organoazides easily to form uranium-nitrogen multiple bonds with the release of dinitrogen. The extent of ligand reduction dictates the formation of uranium mono-, bis- and tris(imido) products. Spectroscopic and structural characterization of these compounds supports the idea that electrons are stored in the ligand framework and used in subsequent reactivity. Computational analyses of the uranium imido products probed their molecular and electronic structures, which facilitated a comparison between the bonding in the tris(imido) structure and its tris(oxo) analogue.

HIGHLY ENRICHED URANIUM BLEND DOWN PROGRAM AT THE SAVANNAH RIVER SITE PRESENT AND FUTURE

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

Magoulas, V; Charles Goergen, C; Ronald Oprea, R

2008-06-05

The Department of Energy (DOE) and Tennessee Valley Authority (TVA) entered into an Interagency Agreement to transfer approximately 40 metric tons of highly enriched uranium (HEU) to TVA for conversion to fuel for the Browns Ferry Nuclear Power Plant. Savannah River Site (SRS) inventories included a significant amount of this material, which resulted from processing spent fuel and surplus materials. The HEU is blended with natural uranium (NU) to low enriched uranium (LEU) with a 4.95% 235U isotopic content and shipped as solution to the TVA vendor. The HEU Blend Down Project provided the upgrades needed to achieve the productmore » throughput and purity required and provided loading facilities. The first blending to low enriched uranium (LEU) took place in March 2003 with the initial shipment to the TVA vendor in July 2003. The SRS Shipments have continued on a regular schedule without any major issues for the past 5 years and are due to complete in September 2008. The HEU Blend program is now looking to continue its success by dispositioning an additional approximately 21 MTU of HEU material as part of the SRS Enriched Uranium Disposition Project.« less

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.

Determination of uranium in natural waters

USGS Publications Warehouse

Barker, Franklin Butt; Johnson, J.O.; Edwards, K.W.; Robinson, B.P.

1965-01-01

A method is described for the determination of very low concentrations of uranium in water. The method is based on the fluorescence of uranium in a pad prepared by fusion of the dried solids from the water sample with a flux of 10 percent NaF 45.5 percent Na2CO3 , and 45.5 percent K2CO3 . This flux permits use of a low fusion temperature and yields pads which are easily removed from the platinum fusion dishes for fluorescence measurements. Uranium concentrations of less than 1 microgram per liter can be determined on a sample of 10 milliliters, or less. The sensitivity and accuracy of the method are dependent primarily on the purity of reagents used, the stability and linearity of the fluorimeter, and the concentration of quenching elements in the water residue. A purification step is recommended when the fluorescence is quenched by more than 30 percent. Equations are given for the calculation of standard deviations of analyses by this method. Graphs of error functions and representative data are also included.

Recovery of uranium from seawater by immobilized tannin

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

Sakaguchi, T.; Nakajima, A.

1987-06-01

Tannin compounds having multiple adjacent hydroxy groups have an extremely high affinity for uranium. To prevent the leaching of tannins into water and to improve the adsorbing characteristics of these compounds, the authors tried to immobilize tannins. The immobilized tannin has the most favorable features for uranium recovery; high selective adsorption ability to uranium, rapid adsorption rate, and applicability in both column and batch systems. The immobilized tannin can recover uranium from natural seawater with high efficiency. About 2530 ..mu..g uranium is adsorbed per gram of this adsorbent within 22 h. Depending on the concentration in seawater, an enrichment ofmore » up to 766,000-fold within the adsorbent is possible. Almost all uranium adsorbed is easily desorbed with a very dilute acid. Thus, the immobilized tannin can be used repeatedly in the adsorption-desorption process.« less

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

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

Studies on separation and purification of fission (99)Mo from neutron activated uranium aluminum alloy.

PubMed

Rao, Ankita; Kumar Sharma, Abhishek; Kumar, Pradeep; Charyulu, M M; Tomar, B S; Ramakumar, K L

2014-07-01

A new method has been developed for separation and purification of fission (99)Mo from neutron activated uranium-aluminum alloy. Alkali dissolution of the irradiated target (100mg) results in aluminum along with (99)Mo and a few fission products passing into solution, while most of the fission products, activation products and uranium remain undissolved. Subsequent purification steps involve precipitation of aluminum as Al(OH)3, iodine as AgI/AgIO3 and molybdenum as Mo-α-benzoin oxime. Ruthenium is separated by volatilization as RuO4 and final purification of (99)Mo was carried out using anion exchange method. The radiochemical yield of fission (99)Mo was found to be >80% and the purity of the product was in conformity with the international pharmacopoeia standards. Copyright © 2014 Elsevier Ltd. All rights reserved.

Analysis by Activation. Part III. Simultaneous Determination of Copper and Uranium in Minerals by Radioactivation; ANALISES POR ATIVACAO. PARTE III. DETERMINACAO SIMULTANEA DE OURO E URANIC NOS MINERAIS POR RADIOATIVACAO

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

Abrao, A.

1959-04-01

ABS>Copper and uranium frequently associated in the same mineral, can be qualitatively and quantitatlvely determined by means of the radioisotopes Au/sup 198/ and Np/sup 239/ formed during the irradiation of the mineral in a reactor The copper is separated from the neptunium and fission products by anion resin without the addition of isotopic carriers. The efficiency of the chemical separation and the purity of the two radioisotopes is controlled by gamma spectroscopy and bidetermination of the half lives. (tr-auth)

High density dispersion fuel

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

Hofman, G.L.

1996-09-01

A fuel development campaign that results in an aluminum plate-type fuel of unlimited LEU burnup capability with an uranium loading of 9 grams per cm{sup 3} of meat should be considered an unqualified success. The current worldwide approved and accepted highest loading is 4.8 g cm{sup {minus}3} with U{sub 3}Si{sub 2} as fuel. High-density uranium compounds offer no real density advantage over U{sub 3}Si{sub 2} and have less desirable fabrication and performance characteristics as well. Of the higher-density compounds, U{sub 3}Si has approximately a 30% higher uranium density but the density of the U{sub 6}X compounds would yield the factormore » 1.5 needed to achieve 9 g cm{sup {minus}3} uranium loading. Unfortunately, irradiation tests proved these peritectic compounds have poor swelling behavior. It is for this reason that the authors are turning to uranium alloys. The reason pure uranium was not seriously considered as a dispersion fuel is mainly due to its high rate of growth and swelling at low temperatures. This problem was solved at least for relatively low burnup application in non-dispersion fuel elements with small additions of Si, Fe, and Al. This so called adjusted uranium has nearly the same density as pure {alpha}-uranium and it seems prudent to reconsider this alloy as a dispersant. Further modifications of uranium metal to achieve higher burnup swelling stability involve stabilization of the cubic {gamma} phase at low temperatures where normally {alpha} phase exists. Several low neutron capture cross section elements such as Zr, Nb, Ti and Mo accomplish this in various degrees. The challenge is to produce a suitable form of fuel powder and develop a plate fabrication procedure, as well as obtain high burnup capability through irradiation testing.« less

URANIUM EXTRACTION PROCESS USING SYNERGISTIC REAGENTS

DOEpatents

Schmitt, J.M.; Blake, C.A. Jr.; Brown, K.B.; Coleman, C.F.

1958-11-01

Improved methods are presented for recovering uranium values from aqueous solutions by organic solvent extraction. The improvement lies in the use, in combination, of two classes of organic compounds so that their extracting properties are enhanced synergistically. The two classes of organic compounds are dialkylphosphoric acid and certain neutral organophosphorus compounds such as trialkylphosphates, trialkylphosphonates, trlalkylphosphinates and trialkylphosphine oxides.

The role of uranium-arene bonding in H2O reduction catalysis

NASA Astrophysics Data System (ADS)

Halter, Dominik P.; Heinemann, Frank W.; Maron, Laurent; Meyer, Karsten

2018-03-01

The reactivity of uranium compounds towards small molecules typically occurs through stoichiometric rather than catalytic processes. Examples of uranium catalysts reacting with water are particularly scarce, because stable uranyl groups form that preclude the recovery of the uranium compound. Recently, however, an arene-anchored, electron-rich uranium complex has been shown to facilitate the electrocatalytic formation of H2 from H2O. Here, we present the precise role of uranium-arene δ bonding in intermediates of the catalytic cycle, as well as details of the atypical two-electron oxidative addition of H2O to the trivalent uranium catalyst. Both aspects were explored by synthesizing mid- and high-valent uranium-oxo intermediates and by performing comparative studies with a structurally related complex that cannot engage in δ bonding. The redox activity of the arene anchor and a covalent δ-bonding interaction with the uranium ion during H2 formation were supported by density functional theory analysis. Detailed insight into this catalytic system may inspire the design of ligands for new uranium catalysts.

Apparatus to recover tritium from tritiated molecules

DOEpatents

Swansiger, William A.

1988-01-01

An apparatus for recovering tritium from tritiated compounds is provided, including a preheater for heating tritiated water and other co-injected tritiated compounds to temperatures of about 600.degree. C. and a reactor charged with a mixture of uranium and uranium dioxide for receiving the preheated mixture. The reactor vessel is preferably stainless steel of sufficient mass so as to function as a heat sink preventing the reactor side walls from approaching high temperatures. A disposable copper liner extends between the reaction chamber and stainless steel outer vessel to prevent alloying of the uranium with the outer vessel. The uranium dioxide functions as an insulating material and heat sink preventing the reactor side walls from attaining reaction temperatures to thereby minimize tritium permeation rates. The uranium dioxide also functions as a diluent to allow for volumetric expansion of the uranium as it is converted to uranium dioxide.

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.

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.

Floquet Topological Insulators in Uranium Compounds

NASA Astrophysics Data System (ADS)

Pi, Shu-Ting; Savrasov, Sergey

2014-03-01

A major issue regarding the Uranium based nuclear fuels is to conduct the heat from the core area to its outer area. Unfortunately, those materials are notorious for their extremely low thermal conductivity due to the phonon-dominated-heat-transport properties in insulating states. Although metallic Uranium compounds are helpful in increasing the thermal conductivity, their low melting point still make those efforts in vain. In this report, we will figure out potential Uranium based Floquet topological insulators where the insulating bulk states accompanied with metallic surface states is achieved by applying periodic electrical fields which makes the coexistence of both benefits possible.

Analysis of a Uranium Oxide Sample Interdicted in Slovakia (FSC 12-3-1)

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

Borg, Lars E.; Dai, Zurong; Eppich, Gary R.

2014-01-17

We provide a concise summary of analyses of a natural uranium sample seized in Slovakia in November 2007. Results are presented for compound identification, water content, U assay, trace element abundances, trace organic compounds, isotope compositions for U, Pb, Sr and O, and age determination using the 234U – 230Th and 235U – 231Pa chronometers. The sample is a mixture of two common uranium compounds - schoepite and uraninite. The uranium isotope composition is indistinguishable from natural; 236U was not detected. The O, Sr and Pb isotope compositions and trace element abundances are unremarkable. The 234U – 230Th chronometer givesmore » an age of 15.5 years relative to the date of analysis, indicating the sample was produced in January 1997. A comparison of the data for this sample with data in the Uranium Sourcing database failed to find a match, indicating the sample was not produced at a facility represented in the database.« less

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.

Radiation shielding materials and containers incorporating same

DOEpatents

Mirsky, Steven M.; Krill, Stephen J.; Murray, Alexander P.

2005-11-01

An improved radiation shielding material and storage systems for radioactive materials incorporating the same. The PYRolytic Uranium Compound ("PYRUC") shielding material is preferably formed by heat and/or pressure treatment of a precursor material comprising microspheres of a uranium compound, such as uranium dioxide or uranium carbide, and a suitable binder. The PYRUC shielding material provides improved radiation shielding, thermal characteristic, cost and ease of use in comparison with other shielding materials. The shielding material can be used to form containment systems, container vessels, shielding structures, and containment storage areas, all of which can be used to house radioactive waste. The preferred shielding system is in the form of a container for storage, transportation, and disposal of radioactive waste. In addition, improved methods for preparing uranium dioxide and uranium carbide microspheres for use in the radiation shielding materials are also provided.

PROCESSES OF RECOVERING URANIUM FROM A CALUTRON

DOEpatents

Baird, D.O.; Zumwalt, L.R.

1958-07-15

An improved process is described for recovering the residue of a uranium compound which has been subjected to treatment in a calutron, from the parts of the calutron disposed in the source region upon which the residue is deposited. The process may be utilized when the uranium compound adheres to a surface containing metals of the group consisting of copper, iron, chromium, and nickel. The steps comprise washing the surface with an aqueous acidic oxidizing solvent for the uranium whereby there is obtained an acidic aqueous Solution containing uranium as uranyl ions and metals of said group as impurities, treating the acidic solution with sodium acetate in the presenee of added sodium nitrate to precipitate the uranium as sodium uranyl acetate away from the impurities in the solution, and separating the sodium uranyl acetate from the solution.

Radiation Shielding Materials and Containers Incorporating Same

DOEpatents

Mirsky, Steven M.; Krill, Stephen J.; and Murray, Alexander P.

2005-11-01

An improved radiation shielding material and storage systems for radioactive materials incorporating the same. The PYRolytic Uranium Compound (''PYRUC'') shielding material is preferably formed by heat and/or pressure treatment of a precursor material comprising microspheres of a uranium compound, such as uranium dioxide or uranium carbide, and a suitable binder. The PYRUC shielding material provides improved radiation shielding, thermal characteristic, cost and ease of use in comparison with other shielding materials. The shielding material can be used to form containment systems, container vessels, shielding structures, and containment storage areas, all of which can be used to house radioactive waste. The preferred shielding system is in the form of a container for storage, transportation, and disposal of radioactive waste. In addition, improved methods for preparing uranium dioxide and uranium carbide microspheres for use in the radiation shielding materials are also provided.

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.

PEROXIDE PROCESS FOR SEPARATION OF RADIOACTIVE MATERIALS

DOEpatents

Seaborg, G.T.; Perlman, I.

1958-09-16

reduced state, from hexavalent uranium. It consists in treating an aqueous solution containing such uranium and plutonium ions with sulfate ions in order to form a soluble uranium sulfate complex and then treating the solution with a soluble thorium compound and a soluble peroxide compound in order to ferm a thorium peroxide carrier precipitate which carries down with it the plutonium peroxide present. During this treatment the pH of the solution must be maintained between 2 and 3.

An Ultrastable Heterobimetallic Uranium(IV)/Vanadium(III) Solid Compound Protected by a Redox-Active Phosphite Ligand: Crystal Structure, Oxidative Dissolution, and First-Principles Simulation.

PubMed

Gui, Daxiang; Dai, Xing; Zheng, Tao; Wang, Xiangxiang; Silver, Mark A; Chen, Lanhua; Zhang, Chao; Diwu, Juan; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao

2018-02-05

The first heterobimetallic uranium(IV)/vanadium(III) phosphite compound, Na 2 UV 2 (HPO 3 ) 6 (denoted as UVP), was synthesized via an in situ redox-active hydrothermal reaction. It exhibits superior hydrolytic and antioxidant stability compared to the majority of structures containing low-valent uranium or vanadium, further elucidated by first-principles simulations, and therefore shows potential applications in nuclear waste management.

ANALYTICAL METHOD FOR THE DETERMINATION OF BORON IN URANYL NITRATE SOLUTIONS

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

None

1962-01-01

A method was developed for the determination of boron in uranyl nitrate solutions. The boron is separated from uranium and other impurities by distillation of methyl borate. It is determined absorptiometrically by means of curcumin in the presence of orthochlorophenol, perchloric acid, and acetic anhydride. The limit of detection is judged to be not greater than 0.05 mu g, but is dependent on the purity of the reagents used. The coefficient of variation on 210 results at the 0.2 mu g boron level was 26% with a bias of -25%. The method may be applied to depleted uranyl nitrate solutionsmore » and uranium slag recovery liquors. (auth)« less

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

[Separation of gamma linolenic acid from evening primrose oil with urea inclusion--orthogonal experiment of optimizing technological parameters and observation of urea inclusion compound I].

PubMed

Wang, Hua; Ling, Man; Xue, Gang; Liu, Fengxia; Guo, Shuxian

2010-05-01

The influence on the urea inclusion compound under different conditions (allocated proportion, time of inclusion, temperature of inclusion) were studied through the orthogonal test, and theoretical reference of urea inclusion process for further optimization wound be offered. The orthogonal experiment was adopted, and microscope was used to observe the shape, aperture size of the urea inclusion compound under different technological parameters, the GC was employed to inspect the purity of GLA. The results indicated that the ratio of fatty acids and urea, inclusion of temperature, time of inclusion had great effect on urea inclusion compound. The three factors and its interactions significantly affected the purity of GLA. The results also showed that the best process was that the ratio of fatty acids and urea was 1 : 3, temperature of inclusion was--15 degrees C, time of inclusion was 24 h. Under the best condition, the purity of GLA reach up to 95.575 9%; and it is feasible to observe the shape and the amount of the urea inclusion compound to reflect and guide the urea inclusion technology.

Chemical state of fission products in irradiated uranium carbide fuel

NASA Astrophysics Data System (ADS)

Arai, Yasuo; Iwai, Takashi; Ohmichi, Toshihiko

1987-12-01

The chemical state of fission products in irradiated uranium carbide fuel has been estimated by equilibrium calculation using the SOLGASMIX-PV program. Solid state fission products are distributed to the fuel matrix, ternary compounds, carbides of fission products and intermetallic compounds among the condensed phases appearing in the irradiated uranium carbide fuel. The chemical forms are influenced by burnup as well as stoichiometry of the fuel. The results of the present study almost agree with the experimental ones reported for burnup simulated carbides.

Grain Size and Phase Purity Characterization of U 3Si 2 Pellet Fuel

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

Hoggan, Rita E.; Tolman, Kevin R.; Cappia, Fabiola

Characterization of U 3Si 2 fresh fuel pellets is important for quality assurance and validation of the finished product. Grain size measurement methods, phase identification methods using scanning electron microscopes equipped with energy dispersive spectroscopy and x-ray diffraction, and phase quantification methods via image analysis have been developed and implemented on U 3Si 2 pellet samples. A wide variety of samples have been characterized including representative pellets from an initial irradiation experiment, and samples produced using optimized methods to enhance phase purity from an extended fabrication effort. The average grain size for initial pellets was between 16 and 18 µm.more » The typical average grain size for pellets from the extended fabrication was between 20 and 30 µm with some samples exhibiting irregular grain growth. Pellets from the latter half of extended fabrication had a bimodal grain size distribution consisting of coarsened grains (>80 µm) surrounded by the typical (20-30 µm) grain structure around the surface. Phases identified in initial uranium silicide pellets included: U 3Si 2 as the main phase composing about 80 vol. %, Si rich phases (USi and U 5Si 4) composing about 13 vol. %, and UO 2 composing about 5 vol. %. Initial batches from the extended U 3Si 2 pellet fabrication had similar phases and phase quantities. The latter half of the extended fabrication pellet batches did not contain Si rich phases, and had between 1-5% UO 2: achieving U 3Si 2 phase purity between 95 vol. % and 98 vol. % U 3Si 2. The amount of UO 2 in sintered U 3Si 2 pellets is correlated to the length of time between U 3Si 2 powder fabrication and pellet formation. These measurements provide information necessary to optimize fabrication efforts and a baseline for future work on this fuel compound.« less

Production of extreme-purity aluminum and silicon by fractional crystallization processing

NASA Astrophysics Data System (ADS)

Dawless, R. K.; Troup, R. L.; Meier, D. L.; Rohatgi, A.

1988-06-01

Large scale fractional crystallization is used commercially at Alcoa to produce extreme purity aluminum (99.999+% Al). The primary market is sputtering targets used to make interconnects for integrated circuits. For some applications the impurities uranium and thorium are reduced to less than 1 ppbw to avoid "soft errors" associated with α particle emission. The crystallization process achieves segregation coefficients which are close to theoretical at normal yields, and this, coupled with the scale of the units, allows practical production of this material. The silicon purification process involves crystallization of Si from molten aluminum alloys containing about 30% silicon. The crystallites from this process are further treated to remove residual Al and an extreme purity ingot is obtained. This material is considered suitable for single crystal or ribbon type photovoltaic cells and for certain IC applications, including highly doped substrates used for epitaxial growth. In production of both extreme purity Al and Si, impurities are rejected to the remaining melt as the crystals form and some separation is achieved by draining this downgraded melt from the unit. Purification of this downgrade by crystallization has also been demonstrated for both systems and is important for achieving high recoveries.

Simulation of uranium and plutonium oxides compounds obtained in plasma

NASA Astrophysics Data System (ADS)

Novoselov, Ivan Yu.; Karengin, Alexander G.; Babaev, Renat G.

2018-03-01

The aim of this paper is to carry out thermodynamic simulation of mixed plutonium and uranium oxides compounds obtained after plasma treatment of plutonium and uranium nitrates and to determine optimal water-salt-organic mixture composition as well as conditions for their plasma treatment (temperature, air mass fraction). Authors conclude that it needs to complete the treatment of nitric solutions in form of water-salt-organic mixtures to guarantee energy saving obtainment of oxide compounds for mixed-oxide fuel and explain the choice of chemical composition of water-salt-organic mixture. It has been confirmed that temperature of 1200 °C is optimal to practice the process. Authors have demonstrated that condensed products after plasma treatment of water-salt-organic mixture contains targeted products (uranium and plutonium oxides) and gaseous products are environmental friendly. In conclusion basic operational modes for practicing the process are showed.

Recycling/Disposal Alternatives for Depleted Uranium Wastes

DTIC Science & Technology

1981-01-01

could pass before new sites are available. Recent experi- ence with attempts to dispose of wastes generated by cleanup of the Three Mile Island...commercial sector. Nonordnance uses include counterweights, Lallast, shielding , and special appli- cations machinery. Although the purity requirements...Refer- ence 11). Since the activity of the tailings is higher than allow- able for unrestricted access, large earth -dam retention systems, known as

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.

Purity of synthetic cannabinoids sold online for recreational use.

PubMed

Ginsburg, Brett C; McMahon, Lance R; Sanchez, Jesus J; Javors, Martin A

2012-01-01

The recreational use of synthetic cannabinoids has recently increased. This increase is due, in part, to the recent availability of inexpensive compound sold legally online in bulk. In particular, JWH-018 (1-pentyl-3-(1-naphthoyl)indole) and JWH-073 (1-butyl-3-(1-naphthoyl)indole) have been found in herbal blends marketed as alternatives to cannabis. Although these particular compounds have recently been emergency scheduled in the United States, online suppliers have shifted sales to other, similar compounds that are not currently scheduled. However, the purity of the drugs obtained from online suppliers is not known. Relative purity of JWH-018 and JWH-073 from three different online suppliers was determined using high-performance liquid chromatography with ultraviolet detection and validated standards obtained from a traditional research chemical supplier. Our results show that JWH-018 and JWH-073 obtained from online vendors was of comparable purity to validated standards, even though the physical properties varied in color, texture, and odor. It is concluded that adverse events following consumption of synthetic cannabinoid preparations is unlikely to be due to impurities or residue from the manufacturing process, but rather to effects of the active drug or interactions with other psychoactive chemicals from herbs blended into products marketed as cannabis alternatives.

Oxygen potential of uranium--plutonium oxide as determined by controlled- atmosphere thermogravimetry

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

Swanson, Gerald C.

1975-10-01

The oxygen-to-metal atom ratio, or O/M, of solid solution uranium- plutonium oxide reactor fuel is a measure of the concentration of crystal defects in the oxide which affect many fuel properties, particularly, fuel oxygen potential. Fabrication of a high-temperature oxygen electrode, employing an electro-active tip of oxygen-deficient solid-state electrolyte, intended to confirm gaseous oxygen potentials is described. Uranium oxide and plutonium oxide O/M reference materials were prepared by in situ oxidation of high purity metals in the thermobalance. A solid solution uranium-plutonium oxide O/M reference material was prepared by alloying the uranium and plutonium metals in a yttrium oxide cruciblemore » at 1200°C and oxidizing with moist He at 250°C. The individual and solid solution oxides were isothermally equilibrated with controlled oxygen potentials between 800 and 1300°C and the equilibrated O/ M ratios calculated with corrections for impurities and buoyancy effects. Use of a reference oxygen potential of -100 kcal/mol to produce an O/M of 2.000 is confirmed by these results. However, because of the lengthy equilibration times required for all oxides, use of the O/M reference materials rather than a reference oxygen potential is recommended for O/M analysis methods calibrations.« less

URANIUM BISMUTHIDE DISPERSION IN MOLTEN METAL

DOEpatents

Teitel, R.J.

1959-10-27

The formation of intermetallic bismuth compounds of thorium or uranium dispersed in a liquid media containing bismuth and lead is described. A bismuthide of uranium dispersed in a liquid metal medium is formed by dissolving uranium in composition of lead and bismuth containing less than 80% lead and lowering the temperature of the composition to a temperature below the point at which the solubility of uranium is exceeded and above the melting point of the composition.

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.

49 CFR 176.84 - Other requirements for stowage and segregation for cargo vessels and passenger vessels.

Code of Federal Regulations, 2014 CFR

2014-10-01

...” flammable liquids. 29 Stow “away from” ammonium compounds. 30 Stow “away from” animal or vegetable oils. 31... vegetable oils. 55 Stow “separated from” ammonia. 56 Stow “separated from” ammonium compounds. 57 Stow... hexahydrate solution, uranium metal hexahydrate solution, uranium metal pyrophoric and thorium metal...

49 CFR 176.84 - Other requirements for stowage and segregation for cargo vessels and passenger vessels.

Code of Federal Regulations, 2013 CFR

2013-10-01

...” flammable liquids. 29 Stow “away from” ammonium compounds. 30 Stow “away from” animal or vegetable oils. 31... vegetable oils. 55 Stow “separated from” ammonia. 56 Stow “separated from” ammonium compounds. 57 Stow... hexahydrate solution, uranium metal hexahydrate solution, uranium metal pyrophoric and thorium metal...

Fluorination process using catalyst

DOEpatents

Hochel, Robert C.; Saturday, Kathy A.

1985-01-01

A process for converting an actinide compound selected from the group consisting of uranium oxides, plutonium oxides, uranium tetrafluorides, plutonium tetrafluorides and mixtures of said oxides and tetrafluorides, to the corresponding volatile actinide hexafluoride by fluorination with a stoichiometric excess of fluorine gas. The improvement involves conducting the fluorination of the plutonium compounds in the presence of a fluoride catalyst selected from the group consisting of CoF.sub.3, AgF.sub.2 and NiF.sub.2, whereby the fluorination is significantly enhanced. The improvement also involves conducting the fluorination of one of the uranium compounds in the presence of a fluoride catalyst selected from the group consisting of CoF.sub.3 and AgF.sub.2, whereby the fluorination is significantly enhanced.

Fluorination process using catalysts

DOEpatents

Hochel, R.C.; Saturday, K.A.

1983-08-25

A process is given for converting an actinide compound selected from the group consisting of uranium oxides, plutonium oxides, uranium tetrafluorides, plutonium tetrafluorides and mixtures of said oxides and tetrafluorides, to the corresponding volatile actinide hexafluoride by fluorination with a stoichiometric excess of fluorine gas. The improvement involves conducting the fluorination of the plutonium compounds in the presence of a fluoride catalyst selected from the group consisting of CoF/sub 3/, AgF/sub 2/ and NiF/sub 2/, whereby the fluorination is significantly enhanced. The improvement also involves conducting the fluorination of one of the uranium compounds in the presence of a fluoride catalyst selected from the group consisting of CoF/sub 3/ and AgF/sub 2/, whereby the fluorination is significantly enhanced.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Uranium carbide fission target R&D for RIA - an update

NASA Astrophysics Data System (ADS)

Greene, J. P.; Levand, A.; Nolen, J.; Burtseva, T.

2004-12-01

For the Rare Isotope Accelerator (RIA) facility, ISOL targets employing refractory compounds of uranium are being developed to produce radioactive ions for post-acceleration. The availability of refractory uranium compounds in forms that have good thermal conductivity, relatively high density, and adequate release properties for short-lived isotopes remains an important issue. Investigations using commercially obtained uranium carbide material and prepared into targets involving various binder materials have been carried out at ANL. Thin sample pellets have been produced for measurements of thermal conductivity using a new method based on electron bombardment with the thermal radiation observed using a two-color optical pyrometer and performed on samples as a function of grain size, pressing pressure and sintering temperature. Manufacture of uranium carbide powder has now been achieved at ANL. Simulations have been carried out on the thermal behavior of the secondary target assembly incorporating various heat shield configurations.

Trivalent uranium phenylchalcogenide complexes: exploring the bonding and reactivity with CS2 in the Tp*2UEPh series (E = O, S, Se, Te).

PubMed

Matson, Ellen M; Breshears, Andrew T; Kiernicki, John J; Newell, Brian S; Fanwick, Phillip E; Shores, Matthew P; Walensky, Justin R; Bart, Suzanne C

2014-12-15

The trivalent uranium phenylchalcogenide series, Tp*2UEPh (Tp* = hydrotris(3,5-dimethylpyrazolyl)borate, E = O (1), S (2), Se (3), Te (4)), has been synthesized to investigate the nature of the U-E bond. All compounds have been characterized by (1)H NMR, infrared and electronic absorption spectroscopies, and in the case of 4, X-ray crystallography. Compound 4 was also studied by SQUID magnetometry. Computational studies establish Mulliken spin densities for the uranium centers ranging from 3.005 to 3.027 (B3LYP), consistent for uranium-chalcogenide bonds that are primarily ionic in nature, with a small covalent contribution. The reactivity of 2-4 toward carbon disulfide was also investigated and showed reversible CS2 insertion into the U(III)-E bond, forming Tp*2U(κ(2)-S2CEPh) (E = S (5), Se (6), Te (7)). Compound 5 was characterized crystallographically.

PROCESS FOR THE PRODUCTION OF AMMONIUM URANIUM FLUORIDE

DOEpatents

Ellis, A.S.; Mooney, R.B.

1953-08-25

This patent relates to the preparation of ammonium uranium fluoride. The process comprises adding a water soluble fluoride to an aqueous solution of a uranous compound containing an ammonium salt, and isolating the resulting precipitate. This patent relates to the manufacture of uranium tetnafluoride from ammonium uranium fluoride, NH/sub 4/UF/sub 5/. Uranium tetrafluoride is prepared by heating the ammonium uranium fluoride to a temperature at which dissociation occurs with liberation of ammonium fluoride. Preferably the process is carried out under reduced pressure, or in a current of an inert gas.

Purification of Hydrogen

DOEpatents

Newton, A S

1950-12-05

Disclosed is a process for purifying hydrogen containing various gaseous impurities by passing the hydrogen over a large surface of uranium metal at a temperature above the decomposition temperature of uranium hydride, and below the decomposition temperature of the compounds formed by the combination of the uranium with the impurities in the hydrogen.

Uranium silicide pellet fabrication by powder metallurgy for accident tolerant fuel evaluation and irradiation

DOE PAGES

Harp, Jason Michael; Lessing, Paul Alan; Hoggan, Rita Elaine

2015-06-21

In collaboration with industry, Idaho National Laboratory is investigating uranium silicide for use in future light water reactor fuels as a more accident resistant alternative to uranium oxide base fuels. Specifically this project was focused on producing uranium silicide (U 3Si 2) pellets by conventional powder metallurgy with a density greater than 94% of the theoretical density. This work has produced a process to consistently produce pellets with the desired density through careful optimization of the process. Milling of the U 3Si 2 has been optimized and high phase purity U 3Si 2 has been successfully produced. Results are presentedmore » from sintering studies and microstructural examinations that illustrate the need for a finely ground reproducible particle size distribution in the source powder. The optimized process was used to produce pellets for the Accident Tolerant Fuel-1 irradiation experiment. The average density of these pellets was 11.54 ±0.06 g/cm 3. Additional characterization of the pellets by scaning electron microscopy and X-ray diffraction has also been performed. As a result, pellets produced in this work have been encapsulated for irradiation, and irradiation in the Advanced Test Reactor is expected soon.« less

Uranium silicide pellet fabrication by powder metallurgy for accident tolerant fuel evaluation and irradiation

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

Harp, Jason Michael; Lessing, Paul Alan; Hoggan, Rita Elaine

In collaboration with industry, Idaho National Laboratory is investigating uranium silicide for use in future light water reactor fuels as a more accident resistant alternative to uranium oxide base fuels. Specifically this project was focused on producing uranium silicide (U 3Si 2) pellets by conventional powder metallurgy with a density greater than 94% of the theoretical density. This work has produced a process to consistently produce pellets with the desired density through careful optimization of the process. Milling of the U 3Si 2 has been optimized and high phase purity U 3Si 2 has been successfully produced. Results are presentedmore » from sintering studies and microstructural examinations that illustrate the need for a finely ground reproducible particle size distribution in the source powder. The optimized process was used to produce pellets for the Accident Tolerant Fuel-1 irradiation experiment. The average density of these pellets was 11.54 ±0.06 g/cm 3. Additional characterization of the pellets by scaning electron microscopy and X-ray diffraction has also been performed. As a result, pellets produced in this work have been encapsulated for irradiation, and irradiation in the Advanced Test Reactor is expected soon.« less

Processing of uranium oxide and silicon carbide based fuel using polymer infiltration and pyrolysis

NASA Astrophysics Data System (ADS)

Singh, Abhishek K.; Zunjarrao, Suraj C.; Singh, Raman P.

2008-09-01

Ceramic composite pellets consisting of uranium oxide, UO 2, contained within a silicon carbide matrix, were fabricated using a novel processing technique based on polymer infiltration and pyrolysis (PIP). In this process, particles of depleted uranium oxide, in the form of U 3O 8, were dispersed in liquid allylhydridopolycarbosilane (AHPCS), and subjected to pyrolysis up to 900 °C under a continuous flow of ultra high purity argon. The pyrolysis of AHPCS, at these temperatures, produced near-stoichiometric amorphous silicon carbide ( a-SiC). Multiple polymer infiltration and pyrolysis (PIP) cycles were performed to minimize open porosity and densify the silicon carbide matrix. Analytical characterization was conducted to investigate chemical interaction between U 3O 8 and SiC. It was observed that U 3O 8 reacted with AHPCS during the very first pyrolysis cycle, and was converted to UO 2. As a result, final composition of the material consisted of UO 2 particles contained in an a-SiC matrix. The physical and mechanical properties were also quantified. It is shown that this processing scheme promotes uniform distribution of uranium fuel source along with a high ceramic yield of the parent matrix.

Uranium 5f shell in UPd2Al3 and URu2Si2 studied by x-ray magnetic circular dichroism

NASA Astrophysics Data System (ADS)

Yaouanc, A.; Dalmas de Réotier, P.; van der Laan, G.; Hiess, A.; Goulon, J.; Neumann, C.; Lejay, P.; Sato, N.

1998-10-01

We report x-ray magnetic circular dichroism (XMCD) measurements performed at the uranium M4,5 edges in the paramagnetic phase of the heavy fermion superconductors UPd2Al3 and URu2Si2. The analysis of the spectra with the first sum rule yields the orbital moment of the 5f shell for both compounds. The shape of the dichroic spectrum at the M5 edge for the two compounds is qualitatively different: a single lobe is observed for URu2Si2 and two lobes are detected for UPd2Al3. This two lobe structure reflects the strong effect of the interaction of the uranium 5f electrons with their environment in the latter compound.

COATING URANIUM FROM CARBONYLS

DOEpatents

Gurinsky, D.H.; Storrs, S.S.

1959-07-14

Methods are described for making adherent corrosion resistant coatings on uranium metal. According to the invention, the uranium metal is heated in the presence of an organometallic compound such as the carbonyls of nickel, molybdenum, chromium, niobium, and tungsten at a temperature sufficient to decompose the metal carbonyl and dry plate the resultant free metal on the surface of the uranium metal body. The metal coated body is then further heated at a higher temperature to thermally diffuse the coating metal within the uranium bcdy.

METHOD FOR THE REDUCTION OF URANIUM COMPOUNDS

DOEpatents

Cooke, W.H.; Crawford, J.W.C.

1959-05-12

An improved technique of preparing massive metallic uranium by the reaction at elevated temperature between an excess of alkali in alkaline earth metal and a uranium halide, such ss uranium tetrafluoride is presented. The improvement comprises employing a reducing atmosphere of hydrogen or the like, such as coal gas, in the vessel during the reduction stage and then replacing the reducing atmosphere with argon gas prior to cooling to ambient temperature.

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.

Isolation and purification of series bioactive components from Hypericum perforatum L. by counter-current chromatography.

PubMed

Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Xu, Chunming; Ito, Yoichiro

2011-03-01

Counter-current chromatography (CCC) 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. Copyright © 2011 Elsevier B.V. All rights reserved.

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

Microbial reduction of uranium

USGS Publications Warehouse

Lovley, D.R.; Phillips, E.J.P.; Gorby, Y.A.; Landa, E.R.

1991-01-01

REDUCTION of the soluble, oxidized form of uranium, U(VI), to insoluble U(IV) is an important mechanism for the immobilization of uranium in aquatic sediments and for the formation of some uranium ores1-10. U(VI) reduction has generally been regarded as an abiological reaction in which sulphide, molecular hydrogen or organic compounds function as the reductant1,2,5,11. Microbial involvement in U(VI) reduction has been considered to be limited to indirect effects, such as microbial metabolism providing the reduced compounds for abiological U(VI) reduction and microbial cell walls providing a surface to stimulate abiological U(VI) reduction1,12,13. We report here, however, that dissimilatory Fe(III)-reducing microorganisms can obtain energy for growth by electron transport to U(VI). This novel form of microbial metabolism can be much faster than commonly cited abiological mechanisms for U(VI) reduction. Not only do these findings expand the known potential terminal electron acceptors for microbial energy transduction, they offer a likely explanation for the deposition of uranium in aquatic sediments and aquifers, and suggest a method for biological remediation of environments contaminated with uranium.

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

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

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

Jaques, Brian; Butt, Darryl P.; Marx, Brian M.

A carbothermic reduction of the metal oxides in a hydrogen/nitrogen mixed gas stream prior to nitriding in a nitrogen gas stream was used to synthesize uranium nitride at 1500 deg. C, cerium nitride at 1400 deg. C, and dysprosium nitride at 1500 deg. C. Cerium nitride and dysprosium nitride were also synthesized via hydriding and nitriding the metal shavings at 900 deg. C and 1500 deg. C, respectively. Also, a novel ball-milling synthesis route was used to produce cerium nitride and dysprosium nitride from the metal shavings at room temperature. Dysprosium nitride was also produced by reacting the metal shavingsmore » in a high purity nitrogen gas stream at 1300 deg. C. All materials were characterized by phase analysis via X-ray diffraction. Only the high purity materials were further analyzed via chemical analysis to characterize the trace oxygen concentration. (authors)« less

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.

Galvanic cell for processing of used nuclear fuel

DOEpatents

Garcia-Diaz, Brenda L.; Martinez-Rodriguez, Michael J.; Gray, Joshua R.; Olson, Luke C.

2017-02-07

A galvanic cell and methods of using the galvanic cell is described for the recovery of uranium from used nuclear fuel according to an electrofluorination process. The galvanic cell requires no input energy and can utilize relatively benign gaseous fluorinating agents. Uranium can be recovered from used nuclear fuel in the form of gaseous uranium compound such as uranium hexafluoride, which can then be converted to metallic uranium or UO.sub.2 and processed according to known methodology to form a useful product, e.g., fuel pellets for use in a commercial energy production system.

Electrochemical fluorination for processing of used nuclear fuel

DOEpatents

Garcia-Diaz, Brenda L.; Martinez-Rodriguez, Michael J.; Gray, Joshua R.; Olson, Luke C.

2016-07-05

A galvanic cell and methods of using the galvanic cell is described for the recovery of uranium from used nuclear fuel according to an electrofluorination process. The galvanic cell requires no input energy and can utilize relatively benign gaseous fluorinating agents. Uranium can be recovered from used nuclear fuel in the form of gaseous uranium compound such as uranium hexafluoride, which can then be converted to metallic uranium or UO.sub.2 and processed according to known methodology to form a useful product, e.g., fuel pellets for use in a commercial energy production system.

19 CFR 191.26 - Recordkeeping for manufacturing drawback.

Code of Federal Regulations, 2010 CFR

2010-04-01

... is applicable to the imported material. If the material is a compound with other constituents, including impurities, and the purity of the compound in the imported material is shown by satisfactory... entered amount of the material to establish the amount of pure compound. The amount of the element in the...

Synthesis of actinide nitrides, phosphides, sulfides and oxides

DOEpatents

Van Der Sluys, William G.; Burns, Carol J.; Smith, David C.

1992-01-01

A process of preparing an actinide compound of the formula An.sub.x Z.sub.y wherein An is an actinide metal atom selected from the group consisting of thorium, uranium, plutonium, neptunium, and americium, x is selected from the group consisting of one, two or three, Z is a main group element atom selected from the group consisting of nitrogen, phosphorus, oxygen and sulfur and y is selected from the group consisting of one, two, three or four, by admixing an actinide organometallic precursor wherein said actinide is selected from the group consisting of thorium, uranium, plutonium, neptunium, and americium, a suitable solvent and a protic Lewis base selected from the group consisting of ammonia, phosphine, hydrogen sulfide and water, at temperatures and for time sufficient to form an intermediate actinide complex, heating said intermediate actinide complex at temperatures and for time sufficient to form the actinide compound, and a process of depositing a thin film of such an actinide compound, e.g., uranium mononitride, by subliming an actinide organometallic precursor, e.g., a uranium amide precursor, in the presence of an effectgive amount of a protic Lewis base, e.g., ammonia, within a reactor at temperatures and for time sufficient to form a thin film of the actinide compound, are disclosed.

Exploratory Solid-State Synthesis of Uranium Chalcogenides and Mixed Anion Uranium Chalcogenides

NASA Astrophysics Data System (ADS)

Ward, Matthew David

Several uranium chalcogenides and mixed anion uranium chalcogenides have been synthesized by solid-state synthetic methods. Structural determinations were carried out via single-crystal X-ray diffraction. Some of these compounds have been further characterized by magnetic measurements, optical properties measurements, Raman spectroscopy, resistivity measurements, XANES and XPS. Eight compounds of the composition MU8Q17 were synthesized and characterized by single-crystal X-ray diffraction. All of these compounds crystallize in the CrU8S17 structure type. XANES measurements indicate that ScU8S17 contains Sc3+ and must be charge balanced with some amount of U 3+. Two compounds of the composition ATiU3Te9 crystallize as black rectangular plates. From single-crystal magnetic measurements, CsTiU 3Te9 is consistent with antiferromagnetic coupling between magnetic U atoms. The uranium chalcogenide compounds NiUS3 and Cr4US 8 were synthesized from reaction of the elements in various fluxes. NiUS3 crystallizes in the GdFeO3 structure type. Cr 4US8 crystallizes in the orthorhombic space group D - Pnma and its structure is related to that of Li4UF 8. The compounds Rh2U6S15, Cs 2Ti2U6Se15, and Cs2Cr 2U6Se15 crystallize as black prisms in the cubic space group O-Im3m. Magnetic measurements on Cs 2Cr2U6Se15 give a value for the Weiss temperature, θWeiss, of 57.59 K, indicative of ferromagnetic coupling. Black plates of CsScU(Se2)Se3 were synthesized from the reaction of the elements in a CsCl flux. CsScU(Se2)Se 3 crystallizes in the orthorhombic space group D- Cmcm . Magnetic susceptibility measurements on CsScU(Se2)Se 3 indicate three regions of magnetic response. The uranium double salt Cs5[U2(μ-S 2)2Cl8]I crystallizes as red plates. Cs 5[U2(μ-S2)2Cl 8]I displays optical anisotropy with band gap energies of 1.99 eV and 2.08 eV along the [001] and [100] polarizations. The uranium oxychalcogenides U7O2Se12 and Na2Ba2(UO2)S4 were synthesized by intentional oxygen contamination. The structure of U7O 2Se12 is related to the previously reported U7Q 12. Na2Ba2(UO2)S4 contains isolated uranyl polyhedra in which each uranium atom may be assigned an oxidation state of +6. The four uranium(IV) chlorophosphates, UCl4(POCl3), [U2Cl9][PCl4], UCl3(PO2Cl 2), and U2Cl8(POCl3) were synthesized in an effort to synthesize new novel uranyl sulfides. All are unstable, but UCl4(POCl3) is the thermodynamically favorable phase.

A Multireference Density Functional Approach to the Calculation of the Excited States of Uranium Ions

DTIC Science & Technology

2007-03-01

approach. xiv A MULTIREFERENCE DENSITY FUNCTIONAL APPROACH TO THE CALCULATION OF THE EXCITED STATES OF URANIUM IONS I. Introduction Actinide chemistry, in...oxidation state of the uranium atom. Uranium, like most early actinides , can possess a wide range of oxidation states, ranging from +3 to +6, due in part...in predicting the electronic spectra for heavy element compounds. The first difficulty is that relativistic effects for actinides are significant

RECOVERY OF URANIUM FROM PITCHBLENDE

DOEpatents

Ruehle, A.E.

1958-06-24

The decontamination of uranium from molybdenum is described. When acid solutions containing uranyl nitrate are contacted with ether for the purpose of extracting the uranium values, complex molybdenum compounds are coextracted with the uranium and also again back-extracted from the ether with the uranium. This invention provides a process for extracting uranium in which coextraction of molybdenum is avoided. It has been found that polyhydric alcohols form complexes with molybdenum which are preferentially water-soluble are taken up by the ether extractant to only a very minor degree. The preferred embodiment of the process uses mannitol, sorbitol or a mixture of the two as the complexing agent.

Ultra-high vacuum compatible preparation chain for intermetallic compounds

NASA Astrophysics Data System (ADS)

Bauer, A.; Benka, G.; Regnat, A.; Franz, C.; Pfleiderer, C.

2016-11-01

We report the development of a versatile material preparation chain for intermetallic compounds, which focuses on the realization of a high-purity growth environment. The preparation chain comprises an argon glovebox, an inductively heated horizontal cold boat furnace, an arc melting furnace, an inductively heated rod casting furnace, an optically heated floating-zone furnace, a resistively heated annealing furnace, and an inductively heated annealing furnace. The cold boat furnace and the arc melting furnace may be loaded from the glovebox by means of a load-lock permitting to synthesize compounds starting with air-sensitive elements while handling the constituents exclusively in an inert gas atmosphere. All furnaces are all-metal sealed, bakeable, and may be pumped to ultra-high vacuum. We find that the latter represents an important prerequisite for handling compounds with high vapor pressure under high-purity argon atmosphere. We illustrate the operational aspects of the preparation chain in terms of the single-crystal growth of the heavy-fermion compound CeNi2Ge2.

Kinetic study of the thermal decomposition of uranium metaphosphate, U(PO3)4, into uranium pyrophosphate, UP2O7

NASA Astrophysics Data System (ADS)

Yang, Hee-Chul; Kim, Hyung-Ju; Lee, Si-Young; Yang, In-Hwan; Chung, Dong-Yong

2017-06-01

The thermochemical properties of uranium compounds have attracted much interest in relation to thermochemical treatments and the safe disposal of radioactive waste bearing uranium compounds. The characteristics of the thermal decomposition of uranium metaphosphate, U(PO3)4, into uranium pyrophosphate, UP2O7, have been studied from the view point of reaction kinetics and acting mechanisms. A mixture of U(PO3)4 and UP2O7 was prepared from the pyrolysis residue of uranium-bearing spent TBP. A kinetic analysis of the reaction of U(PO3)4 into UP2O7 was conducted using an isoconversional method and a master plot method on the basis of data from a non-isothermal thermogravimetric analysis. The thermal decomposition of U(PO3)4 into UP2O7 followed a single-step reaction with an activation energy of 175.29 ± 1.58 kJ mol-1. The most probable kinetic model was determined as a type of nucleation and nuclei-growth models, the Avrami-Erofeev model (A3), which describes that there are certain restrictions on nuclei growth of UP2O7 during the solid-state decomposition of U(PO3)4.

CHEMICAL DIFFERENCES BETWEEN SLUDGE SOLIDS AT THE F AND H AREA TANK FARMS

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

Reboul, S.

2012-08-29

The primary source of waste solids received into the F Area Tank Farm (FTF) was from PUREX processing performed to recover uranium and plutonium from irradiated depleted uranium targets. In contrast, two primary sources of waste solids were received into the H Area Tank Farm (HTF): a) waste from PUREX processing; and b) waste from H-modified (HM) processing performed to recover uranium and neptunium from burned enriched uranium fuel. Due to the differences between the irradiated depleted uranium targets and the burned enriched uranium fuel, the average compositions of the F and H Area wastes are markedly different from onemore » another. Both F and H Area wastes contain significant amounts of iron and aluminum compounds. However, because the iron content of PUREX waste is higher than that of HM waste, and the aluminum content of PUREX waste is lower than that of HM waste, the iron to aluminum ratios of typical FTF waste solids are appreciably higher than those of typical HTF waste solids. Other constituents present at significantly higher concentrations in the typical FTF waste solids include uranium, nickel, ruthenium, zinc, silver, cobalt and copper. In contrast, constituents present at significantly higher concentrations in the typical HTF waste solids include mercury, thorium, oxalate, and radionuclides U-233, U-234, U-235, U-236, Pu-238, Pu-242, Cm-244, and Cm-245. Because of the higher concentrations of Pu-238 in HTF, the long-term concentrations of Th-230 and Ra-226 (from Pu-238 decay) will also be higher in HTF. The uranium and plutonium distributions of the average FTF waste were found to be consistent with depleted uranium and weapons grade plutonium, respectively (U-235 comprised 0.3 wt% of the FTF uranium, and Pu-240 comprised 6 wt% of the FTF plutonium). In contrast, at HTF, U-235 comprised 5 wt% of the uranium, and Pu-240 comprised 17 wt% of the plutonium, consistent with enriched uranium and high burn-up plutonium. X-ray diffraction analyses of various FTF and HTF samples indicated that the primary crystalline compounds of iron in sludge solids are Fe{sub 2}O{sub 3}, Fe{sub 3}O{sub 4}, and FeO(OH), and the primary crystalline compounds of aluminum are Al(OH){sub 3} and AlO(OH). Also identified were carbonate compounds of calcium, magnesium, and sodium; a nitrated sodium aluminosilicate; and various uranium compounds. Consistent with expectations, oxalate compounds were identified in solids associated with oxalic acid cleaning operations. The most likely oxidation states and chemical forms of technetium are assessed in the context of solubility, since technetium-99 is a key risk driver from an environmental fate and transport perspective. The primary oxidation state of technetium in SRS sludge solids is expected to be Tc(IV). In salt waste, the primary oxidation state is expected to be Tc(VII). The primary form of technetium in sludge is expected to be a hydrated technetium dioxide, TcO{sub 2} {center_dot} xH{sub 2}O, which is relatively insoluble and likely co-precipitated with iron. In salt waste solutions, the primary form of technetium is expected to be the very soluble pertechnetate anion, TcO{sub 4}{sup -}. The relative differences between the F and H Tank Farm waste provide a basis for anticipating differences that will occur as constituents of FTF and HTF waste residue enter the environment over the long-term future. If a constituent is significantly more dominant in one of the Tank Farms, its long-term environmental contribution will likely be commensurately higher, assuming the environmental transport conditions of the two Tank Farms share some commonality. It is in this vein that the information cited in this document is provided - for use during the generation, assessment, and validation of Performance Assessment modeling results.« less

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.

Reactor Physics Measurements and Benchmark Specifications for Oak Ridge Highly Enriched Uranium Sphere (ORSphere)

DOE PAGES

Marshall, Margaret A.

2014-11-04

In the early 1970s Dr. John T. Mihalczo (team leader), J.J. Lynn, and J.R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) in an effort to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950s. The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared with themore » GODIVA I experiments. Additionally, various material reactivity worths, the surface material worth coefficient, the delayed neutron fraction, the prompt neutron decay constant, relative fission density, and relative neutron importance were all measured. The critical assembly, material reactivity worths, the surface material worth coefficient, and the delayed neutron fraction were all evaluated as benchmark experiment measurements. The reactor physics measurements are the focus of this paper; although for clarity the critical assembly benchmark specifications are briefly discussed.« less

Characteristics of uranium carbonitride microparticles synthesized using different reaction conditions

NASA Astrophysics Data System (ADS)

Silva, Chinthaka M.; Lindemer, Terrence B.; Voit, Stewart R.; Hunt, Rodney D.; Besmann, Theodore M.; Terrani, Kurt A.; Snead, Lance L.

2014-11-01

Three sets of experimental conditions were tested to synthesize uranium carbonitride (UC1-xNx) kernels from gel-derived urania-carbon microspheres. Primarily, three sequences of gases were used, N2 to N2-4%H2 to Ar, Ar to N2 to Ar, and Ar-4%H2 to N2-4%H2 to Ar-4%H2. Physical and chemical characteristics such as geometrical density, phase purity, and chemical compositions of the synthesized UC1-xNx were measured. Single-phase kernels were commonly obtained with densities generally ranging from 85% to 93% TD and values of x as high as 0.99. In-depth analysis of the microstrutures of UC1-xNx has been carried out and is discussed with the objective of large batch fabrication of high density UC1-xNx kernels.

METHOD OF PROCESSING MONAZITE SAND

DOEpatents

Calkins, G.D.

1957-10-29

A method is given for the pretreatment of monazite sand with sodium hydroxide. When momazite sand is reacted with sodium hydroxide, the thorium, uranium, and rare earths are converted to water-insoluble hydrous oxides; but in the case of uranium, the precipitate compound may at least partly consist of a slightly soluble uranate. According to the patent, monazite sand is treated with an excess of aqueous sodium hydroxide solution, and the insoluble compounds of thorium, uranium, and the rare earths are separated from the aqueous solution. This solution is then concentrated causing sodium phosphate to crystallize out. The crystals are removed from the remaining solution, and the solution is recycled for reaction with a mew supply of momazite sand.

NUCLEAR REACTOR FUEL ELEMENT AND METHOD OF MANUFACTURE

DOEpatents

Brooks, H.

1960-04-26

A description is given for a fuel element comprising a body of uranium metal or an uranium compound dispersed in a matrix material made from magnesium, calcium, or barium and a stainless steel jacket enclosing the body.

Reconnaissance for trace elements in North Dakota and eastern Montana. Part 1. Geology and radioactivity. Part 2. Reserves and summary

USGS Publications Warehouse

Wyant, Donald G.; Beroni, Ernest P.

1950-01-01

The exact mode of origin of the uranium in the lignite is not known. Uranium may have accumulated in swamps at the same time as the organic debris, or it may have been introduced by ground water after the formation of lignite. In either case carbon or carbon compounds apparently caused the precipitation or fixation of uranium. Further work is needed to determine the origin of this type of uranium deposit.

LIQUID PHASE SINTERING OF METALLIC CARBIDES

DOEpatents

Hammond, J.; Sease, J.D.

1964-01-21

An improved method is given for fabricating uranium carbide composites, The method comprises forming a homogeneous mixture of powdered uranium carbide, a uranium intermetallic compound which wets and forms a eutectic with said carbide and has a non-uranium component which has a relatively high vapor pressure at a temperature in the range 1200 to 1500 deg C, and an organic binder, pressing said mixture to a composite of desired green strength, and then vacuum sintering said composite at the eutectic forming temperature for a period sufficient to remove at least a portion of the non-uranium containing component of said eutectic. (AEC)

Growth of High Purity Oxygen-Free Silicon by Cold Crucible Techniques.

DTIC Science & Technology

1982-06-01

Liquid Metals (A Review). High Temp.-High Pressures 2(6), 583-586, 1970. 1971 Knights, C.F. and Perkins, R. Levitation Melting of Uranium Mono- Carbide . J...content - typically I PPM or less. c) The crystals grown exhibited a high level of carbon contamination (2-30 PPM ) which we believe, is caused by the...grown from melts confined in the cold crucible exhibit an unusually low oxygen content - typically 1 PPM or less. c.) The crystals grown exhibited a

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.

Process for producing an aggregate suitable for inclusion into a radiation shielding product

DOEpatents

Lessing, Paul A.; Kong, Peter C.

2000-01-01

The present invention is directed to methods for converting depleted uranium hexafluoride to a stable depleted uranium silicide in a one-step reaction. Uranium silicide provides a stable aggregate material that can be added to concrete to increase the density of the concrete and, consequently, shield gamma radiation. As used herein, the term "uranium silicide" is defined as a compound generically having the formula U.sub.x Si.sub.y, wherein the x represents the molecules of uranium and the y represent the molecules of silicon. In accordance with the present invention, uranium hexafluoride is converted to a uranium silicide by contacting the uranium hexafluoride with a silicon-containing material at a temperature in a range between about 1450.degree. C. and about 1750.degree. C. The stable depleted uranium silicide is included as an aggregate in a radiation shielding product, such as a concrete product.

Argon/UF6 plasma exhaust gas reconstitution experiments using preheated fluorine and on-line diagnostics. [fissioning uranium plasma core reactor design

NASA Technical Reports Server (NTRS)

Roman, W. C.

1979-01-01

The feasibility of employing a flowing, high-temperature, pure fluorine/UF6 regeneration system to efficiently convert a large fraction of the effluent plasma exhaust back to pure UF6 was demonstrated. The custom built T.O.F. mass spectrometer sampling system permitted on-line measurements of the UF6 concentration at different locations in the exhaust system. Negligible amounts ( 100 ppm) of UF6 were detected in the axial bypass exhaust duct and the exhaust ducts downstream of the cryogenic trap system used to collect the UF6, thus verifying the overall system efficiency over a range of operating conditions. Use of a porous Monel duct as part of the exhaust duct system, including provision for injection of pure fluorine, provided a viable technique to eliminate uranium compound residue on the inside surface of the exhaust ducts. Typical uranium compound mass deposition per unit area of duct was 2 micron g/sq cm. This porous duct technique is directly applicable to future uranium compound transfer exhaust systems. Throughout these experiments, additional basic data on the corrosion aspects of hot, pressurized UF6/fluorine were also accumulated.

United States-Gulf Cooperation Council Security Cooperation in a Multipolar World

DTIC Science & Technology

2014-10-01

including plu- tonium separation experiments, uranium enrichment and conversion experiments, and importing various uranium compounds.28 Subsequent...against political protest, a status shared with the two other remaining Arab monarchies, Morocco and Jordan . Geopolitically, the GCC as a region has...commitments, the UAE will not enrich uranium itself, relying instead on imported, enriched fuel. “Abu Dhabi Moves Ahead With Nuclear Program,” Middle

Hydrothermal synthesis of (C6N2H14)2(UVI2UIVO4F12), a mixed-valent one-dimensional uranium oxyfluoride.

PubMed

Allen, S; Barlow, S; Halasyamani, P S; Mosselmans, J F; O'Hare, D; Walker, S M; Walton, R I

2000-08-21

A new hybrid organic-inorganic mixed-valent uranium oxyfluoride, (C6N2H14)2(U3O4F12), UFO-17, has been synthesized under hydrothermal conditions using uranium dioxide as the uranium source, hydrofluoric acid as mineralizer, and 1,4-diazabicyclo[2.2.2]octane as template. The single-crystal X-ray structure was determined. Crystals of UFO-17 belonged to the orthorhombic space group Cmcm (no. 63), with a = 14.2660(15) A, b = 24.5130(10) A, c = 7.201(2) A, and Z = 4. The structure reveals parallel uranium-containing chains of two types: one type is composed of edge-sharing UO2F5 units; the other has a backbone of edge-sharing UF8 units, each sharing an edge with a pendant UO2F5 unit. Bond-valence calculations suggest the UF8 groups contain UIV, while the UO2F5 groups contain UVI. EXAFS data give results consistent with the single-crystal X-ray structure determination, while comparison of the uranium LIII-edge XANES of UFO-17 with that of related UIV and UVI compounds supports the oxidation-state assignment. Variable-temperature magnetic susceptibility measurements on UFO-17 and a range of related hybrid organic-inorganic uranium(IV) and uranium(VI) fluorides and oxyfluorides further support the formulation of UFO-17 as a mixed-valent UIV/UVI compound.

Production of metals and compounds by radiation chemistry

NASA Technical Reports Server (NTRS)

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

1969-01-01

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

SEPARATION PROCESS FOR TRANSURANIC ELEMENT AND COMPOUNDS THEREOF

DOEpatents

Calvin, M.

1958-10-14

S> A process is presented for the separation of pluto nium from uranium and fission products in an aqueous acidic solution by use of a chelating agent. The plutonium is maintained in the tetravalent state and the uranium in the hexavalent state, and the acidic concentration is adjusted to about 1 N bar. The aqueous solution is then contacted with a water-immiscible organic solvent solution and the chelating agent. The chelating agents covered by this invention comprise a group of compounds characterized as fluorinated beta-diketones.

Semi-automated potentiometric titration method for uranium characterization.

PubMed

Cristiano, B F G; Delgado, J U; da Silva, J W S; de Barros, P D; de Araújo, R M S; Lopes, R T

2012-07-01

The manual version of the potentiometric titration method has been used for certification and characterization of uranium compounds. In order to reduce the analysis time and the influence of the analyst, a semi-automatic version of the method was developed in the Brazilian Nuclear Energy Commission. The method was applied with traceability assured by using a potassium dichromate primary standard. The combined standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization. Copyright © 2011 Elsevier Ltd. All rights reserved.

FUEL ELEMENTS AND METHOD OF MAKING

DOEpatents

Noland, R.A.; Marzano, C.

1958-08-19

A process is described of surface-impregnating bodies of metallic uranium with silicon. Silicon metal is added to or admixed with alkali metal selected from the group consisting of sodiunn, potassium, and sodiunnpotassium alloy. The uraniunn body is then immersed in the mixture obtained and the temperature is raised to between 425 and 600 deg C. The silicon is dissolved and deposits as a uranium-silicon compound on the uranium body.

METHOD FOR PURIFYING URANIUM

DOEpatents

Kennedy, J.W.; Segre, E.G.

1958-08-26

A method is presented for obtaining a compound of uranium in an extremely pure state and in such a condition that it can be used in determinations of the isotopic composition of uranium. Uranium deposited in calutron receivers is removed therefrom by washing with cold nitric acid and the resulting solution, coataining uranium and trace amounts of various impurities, such as Fe, Ag, Zn, Pb, and Ni, is then subjected to various analytical manipulations to obtain an impurity-free uranium containing solution. This solution is then evaporated on a platinum disk and the residue is ignited converting it to U2/sub 3//sub 8/. The platinum disk having such a thin film of pure U/sub 2/O/sub 8/ is suitable for use with isotopic determination techaiques.

Fission-Produced 99Mo Without a Nuclear Reactor.

PubMed

Youker, Amanda J; Chemerisov, Sergey D; Tkac, Peter; Kalensky, Michael; Heltemes, Thad A; Rotsch, David A; Vandegrift, George F; Krebs, John F; Makarashvili, Vakho; Stepinski, Dominique C

2017-03-01

99 Mo, the parent of the widely used medical isotope 99m Tc, is currently produced by irradiation of enriched uranium in nuclear reactors. The supply of this isotope is encumbered by the aging of these reactors and concerns about international transportation and nuclear proliferation. Methods: We report results for the production of 99 Mo from the accelerator-driven subcritical fission of an aqueous solution containing low enriched uranium. The predominately fast neutrons generated by impinging high-energy electrons onto a tantalum convertor are moderated to thermal energies to increase fission processes. The separation, recovery, and purification of 99 Mo were demonstrated using a recycled uranyl sulfate solution. Conclusion: The 99 Mo yield and purity were found to be unaffected by reuse of the previously irradiated and processed uranyl sulfate solution. Results from a 51.8-GBq 99 Mo production run are presented. © 2017 by the Society of Nuclear Medicine and Molecular Imaging.

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.

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

X-ray magnetic circular dichroism in d and f ferromagnetic materials: recent theoretical progress. Part II (Review Article)

NASA Astrophysics Data System (ADS)

Antonov, V. N.; Shpak, A. P.; Yaresko, A. N.

2008-02-01

The present state of theoretical understanding of the x-ray magnetic circular dichroism (XMCD) of 4f and 5f compounds is reviewed. Energy band theory based upon the local spin-density approximation (LSDA) describes the XMCD spectra of transition metal compounds with high accuracy. However, the LSDA does not suffice for lanthanide compounds which have a correlated 4f shell. A satisfactory description of the XMCD spectra could be obtained by using a generalization of the LSDA, in which explicitly f electron Coulomb correlations are taken into account (LSDA +U approach). As examples of this group we consider the compound GdN. We also consider uranium 5f compounds. In those compounds where the 5f electrons are rather delocalized, the LSDA describes the XMCD spectra reasonably well. As an example of this group we consider UFe2. Particular differences occur for uranium compounds in which the 5f electrons are neither delocalized nor localized, but more or less semilocalized. Typical examples are UXAl (X =Co, Rh, and Pt), and UX (X =S, Se, Te). However, the semilocalized 5f's are not inert, but their interaction with conduction electrons plays an important role. We also consider the electronic structure and XMCD spectra of the heavy-fermion compounds UPt3, URu2Si2, UPd2Al3, UNi2Al3, and UBe13, where the degree of the 5f localization is increased in comparison with other uranium compounds. The electronic structure and XMCD spectra of UGe2 which possesses simultaneously ferromagnetism and superconductivity also presented. Recently achieved improvements for describing 5f compounds are discussed.

Compound Nucleus Reactions in LENR, Analogy to Uranium Fission

NASA Astrophysics Data System (ADS)

Hora, Heinrich; Miley, George; Philberth, Karl

2008-03-01

The discovery of nuclear fission by Hahn and Strassmann was based on a very rare microanalytical result that could not initially indicate the very complicated details of this most important process. A similarity is discussed for the low energy nuclear reactions (LENRs) with analogies to the yield structure found in measurements of uranium fission. The LENR product distribution measured earlier in a reproducible way in experiments with thin film electrodes and a high density deuteron concentration in palladium has several striking similarities with the uranium fission fragment yield curve.ootnotetextG.H. Miley and J.A. Patterson, J. New Energy 1, 11 (1996); G.H. Miley et al, Proc ICCF6, p. 629 (1997).This comparison is specifically focussed to the Maruhn-Greiner local maximum of the distribution within the large-scale minimum when the fission nuclei are excited. Implications for uranium fission are discussed in comparison with LENR relative to the identification of fission a hypothetical compound nuclear reaction via a element ^306X126 with double magic numbers.

Method and apparatus for hydrogen production from water

NASA Technical Reports Server (NTRS)

Muradov, Nazim Z. (Inventor)

2012-01-01

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

High temperature UF6 RF plasma experiments applicable to uranium plasma core reactors

NASA Technical Reports Server (NTRS)

Roman, W. C.

1979-01-01

An investigation was conducted using a 1.2 MW RF induction heater facility to aid in developing the technology necessary for designing a self critical fissioning uranium plasma core reactor. Pure, high temperature uranium hexafluoride (UF6) was injected into an argon fluid mechanically confined, steady state, RF heated plasma while employing different exhaust systems and diagnostic techniques to simulate and investigate some potential characteristics of uranium plasma core nuclear reactors. The development of techniques and equipment for fluid mechanical confinement of RF heated uranium plasmas with a high density of uranium vapor within the plasma, while simultaneously minimizing deposition of uranium and uranium compounds on the test chamber peripheral wall, endwall surfaces, and primary exhaust ducts, is discussed. The material tests and handling techniques suitable for use with high temperature, high pressure, gaseous UF6 are described and the development of complementary diagnostic instrumentation and measurement techniques to characterize the uranium plasma, effluent exhaust gases, and residue deposited on the test chamber and exhaust system components is reported.

Model of a Generic Natural Uranium Conversion Plant ? Suggested Measures to Strengthen International Safeguards

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

Raffo-Caiado, Ana Claudia; Begovich, John M; Ferrada, Juan J

This is the final report that closed a joint collaboration effort between DOE and the National Nuclear Energy Commission of Brazil (CNEN). In 2005, DOE and CNEN started a collaborative effort to evaluate measures that can strengthen the effectiveness of international safeguards at a natural uranium conversion plant (NUCP). The work was performed by DOE s Oak Ridge National Laboratory and CNEN. A generic model of a NUCP was developed and typical processing steps were defined. Advanced instrumentation and techniques for verification purposes were identified and investigated. The scope of the work was triggered by the International Atomic Energy Agencymore » s 2003 revised policy concerning the starting point of safeguards at uranium conversion facilities. Prior to this policy only the final products of the uranium conversion plant were considered to be of composition and purity suitable for use in the nuclear fuel cycle and therefore, subject to the IAEA safeguards control. DOE and CNEN have explored options for implementing the IAEA policy, although Brazil understands that the new policy established by the IAEA is beyond the framework of the Quadripartite Agreement of which it is one of the parties, together with Argentina, the Brazilian-Argentine Agency for Accounting and Control of Nuclear Materials (ABACC) and the IAEA. Two technical papers on this subject were published at the 2005 and 2008 INMM Annual Meetings.« less

The application of visible absorption spectroscopy to the analysis of uranium in aqueous solutions

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

Colletti, Lisa Michelle; Copping, Roy; Garduno, Katherine

Through assay analysis into an excess of 1 M H 2SO 4 at fixed temperature a technique has been developed for uranium concentration analysis by visible absorption spectroscopy over an assay concentration range of 1.8 – 13.4 mgU/g. Once implemented for a particular spectrophotometer and set of spectroscopic cells this technique promises to provide more rapid results than a classical method such as Davies-Gray (DG) titration analysis. While not as accurate and precise as the DG method, a comparative analysis study reveals that the spectroscopic method can analyze for uranium in well characterized uranyl(VI) solution samples to within 0.3% ofmore » the DG results. For unknown uranium solutions in which sample purity is less well defined agreement between the developed spectroscopic method and DG analysis is within 0.5%. The technique can also be used to detect the presence of impurities that impact the colorimetric analysis, as confirmed through the analysis of ruthenium contamination. Finally, extending the technique to other assay solution, 1 M HNO 3, HCl and Na 2CO 3, has also been shown to be viable. As a result, of the four aqueous media the carbonate solution yields the largest molar absorptivity value at the most intensely absorbing band, with the least impact of temperature.« less

The application of visible absorption spectroscopy to the analysis of uranium in aqueous solutions

DOE PAGES

Colletti, Lisa Michelle; Copping, Roy; Garduno, Katherine; ...

2017-07-18

Through assay analysis into an excess of 1 M H 2SO 4 at fixed temperature a technique has been developed for uranium concentration analysis by visible absorption spectroscopy over an assay concentration range of 1.8 – 13.4 mgU/g. Once implemented for a particular spectrophotometer and set of spectroscopic cells this technique promises to provide more rapid results than a classical method such as Davies-Gray (DG) titration analysis. While not as accurate and precise as the DG method, a comparative analysis study reveals that the spectroscopic method can analyze for uranium in well characterized uranyl(VI) solution samples to within 0.3% ofmore » the DG results. For unknown uranium solutions in which sample purity is less well defined agreement between the developed spectroscopic method and DG analysis is within 0.5%. The technique can also be used to detect the presence of impurities that impact the colorimetric analysis, as confirmed through the analysis of ruthenium contamination. Finally, extending the technique to other assay solution, 1 M HNO 3, HCl and Na 2CO 3, has also been shown to be viable. As a result, of the four aqueous media the carbonate solution yields the largest molar absorptivity value at the most intensely absorbing band, with the least impact of temperature.« less

THE CHEMICAL ANALYSIS OF TERNARY ALLOYS OF PLUTONIUM WITH MOLYBDENUM AND URANIUM

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

Phillips, G.; Woodhead, J.; Jenkins, E.N.

1958-09-01

It is shown that the absorptiometric determination of molybdenum as thiocyanate may be used in the presence of plutonium. Molybdenum interferes with previously published methods for determining uranium and plutonium but conditlons have been established for its complete removal by solvent extraction of the compound with alpha -benzoin oxime. The previous methods for uranium and plutonium are satisfactory when applied to the residual aqueous phase following this solvent extraction. (auth)

Tc-99 Decontamination From Heat Treated Gaseous Diffusion Membrane -Phase I

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

Oji, L.; Wilmarth, B.; Restivo, M.

2017-03-13

Uranium gaseous diffusion cascades represent a significant environmental challenge to dismantle, containerize and dispose as low-level radioactive waste. Baseline technologies rely on manual manipulations involving direct access to technetium-contaminated piping and materials. There is a potential to utilize novel thermal decontamination technologies to remove the technetium and allow for on-site disposal of the very large uranium converters. Technetium entered these gaseous diffusion cascades as a hexafluoride complex in the same fashion as uranium. Technetium, as the isotope Tc-99, is an impurity that follows uranium in the first cycle of the Plutonium and Uranium Extraction (PUREX) process. The technetium speciation ormore » exact form in the gas diffusion cascades is not well defined. Several forms of Tc-99 compounds, mostly the fluorinated technetium compounds with varying degrees of volatility have been speculated by the scientific community to be present in these cascades. Therefore, there may be a possibility of using thermal desorption, which is independent of the technetium oxidation states, to perform an in situ removal of the technetium as a volatile species and trap the radionuclide on sorbent traps which could be disposed as low-level waste.« less

Rapid extraction and assay of uranium from environmental surface samples

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

Barrett, Christopher A.; Chouyyok, Wilaiwan; Speakman, Robert J.

Extraction methods enabling faster removal and concentration of uranium compounds for improved trace and low-level assay are demonstrated for standard surface sampling material in support of nuclear safeguards efforts, health monitoring, and other nuclear analysis applications. A key problem with the existing surface sampling swipes is the requirement for complete digestion of sample and sampling matrix. This is a time-consuming and labour-intensive process that limits laboratory throughput, elevates costs, and increases background levels. Various extraction methods are explored for their potential to quickly and efficiently remove different chemical forms of uranium from standard surface sampling material. A combination of carbonatemore » and peroxide solutions is shown to give the most rapid and complete form of uranyl compound extraction and dissolution. This rapid extraction process is demonstrated to be compatible with standard inductive coupled plasma mass spectrometry methods for uranium isotopic assay as well as screening techniques such as x-ray fluorescence. The general approach described has application beyond uranium to other analytes of nuclear forensic interest (e.g., rare earth elements and plutonium) as well as heavy metals for environmental and industrial hygiene monitoring.« less

FLUORIDE VOLATILITY PROCESS FOR THE RECOVERY OF URANIUM

DOEpatents

Katz, J.J.; Hyman, H.H.; Sheft, I.

1958-04-15

The separation and recovery of uraniunn from contaminants introduced by neutron irradiation by a halogenation and volatilization method are described. The irradiated uranium is dissolved in bromine trifluoride in the liquid phase. The uranium is converted to the BrF/sub 3/ soluble urmium hexafluoride compound whereas the fluorides of certain contaminating elements are insoluble in liquid BrF/sub 3/, and the reaction rate of the BrF/sub 3/ with certain other solid uranium contamirnnts is sufficiently slower than the reaction rate with uranium that substantial portions of these contaminating elements will remain as solids. These solids are then separated from the solution by a distillation, filtration, or centrifugation step. The uranium hexafluoride is then separated from the balance of the impurities and solvent by one or more distillations.

Dispersion and separation of nanostructured carbon in organic solvents

NASA Technical Reports Server (NTRS)

Evans, Christopher M. (Inventor); Ruf, Herbert J. (Inventor); Landi, Brian J. (Inventor); Raffaelle, Ryne P. (Inventor)

2011-01-01

The present invention relates to dispersions of nanostructured carbon in organic solvents containing alkyl amide compounds and/or diamide compounds. The invention also relates to methods of dispersing nanostructured carbon in organic solvents and methods of mobilizing nanostructured carbon. Also disclosed are methods of determining the purity of nanostructured carbon.

Material Problems for High-Temperature, High-Power Space Energy-Conversion Systems.

DTIC Science & Technology

1984-05-01

M. Takahashi, S. Nanamaku, and M. Kimura , "The growth of ferroelectric single crystal Sr 2 Mb2 0 7 by means of F.Z. technique," J. of Crystal Growth...Holsbeke, "Preparation and characterization of high purity vanadium by EBFZM," J. of Less Common Metals, Vol. 39, 7-16 (1975). 18. S. Takai and H. Kimura ... uranium system from room temperature to 900 0C. The composition of maximum hardness increased from 40 atomic percent (a/o) zirconium at room ’ 69

Hydrometallurgical methods of recovery of scandium from the wastes of various technologies

NASA Astrophysics Data System (ADS)

Molchanova, T. V.; Akimova, I. D.; Smirnov, K. M.; Krylova, O. K.; Zharova, E. V.

2017-03-01

The recovery of scandium from the wastes of the production of uranium, titanium, iron-vanadium, and alumina is studied. The applied acid schemes of scandium transfer to a solution followed by ion-exchange recovery and extraction concentration of scandium ensure the precipitation of crude scandium oxides containing up to 5% Sc2O3. Scandium oxides of 99.96-99.99% purity are formed after additional refining of these crude oxides according to an extraction technology using a mixture 15% multiradical phosphine oxide or Cyanex-925 + 15% tributyl phosphate in kerosene.

SINGLE-STEP CONVERSION OF UO$sub 3$ TO UF$sub 4$

DOEpatents

Moore, J.E.

1960-07-12

A description is given of the preparation of uranium tetrafluoride by reacting a hexavalent uranium compound with a pclysaccharide and gaseous hydrogen fluoride at an elevated temperature. Uranium trioxide and starch are combined with water to form a doughy mixture. which is extruded into pellets and dried. The pellets are then contacted with HF at a temperature from 500 to 700 deg C in a moving bed reactor to prcduce UF/sub 4/. Reduction of the hexavalent uranium to UO/sub 2/ and conversion of the UO/sub 2/ to UF/sub 4/ are accomplished simultaneously in this process.

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

Pro-static Agents in Jet Fuels

DTIC Science & Technology

1976-08-16

1000 10,000 CHARGE DENSITY (juC/ms) Fig. 5- Effect otpolar compounds on charging tendency of silica-gel-treated n-heptane Naphthenic acid is neither a...Eastmant Naphthenic acids Practical Eastman t 30 NRL REPORT 8021 Compound Purity Supplier Pararosandine hydrochloride Not available Eastmant...silica gel to remove moisture and polar contaminants that might interfere with the compound or additive being screened. This treatment Manuscript

Uranium in well drinking water of Kabul, Afghanistan and its effective, low-cost depuration using Mg-Fe based hydrotalcite-like compounds.

PubMed

Kato, Masashi; Azimi, Mohammad Daud; Fayaz, Said Hafizullah; Shah, Muhammad Dawood; Hoque, Md Zahirul; Hamajima, Nobuyuki; Ohnuma, Shoko; Ohtsuka, Tomomi; Maeda, Masao; Yoshinaga, Masafumi

2016-12-01

Toxic elements in drinking water have great effects on human health. However, there is very limited information about toxic elements in drinking water in Afghanistan. In this study, levels of 10 elements (chromium, nickel, copper, arsenic, cadmium, antimony, barium, mercury, lead and uranium) in 227 well drinking water samples in Kabul, Afghanistan were examined for the first time. Chromium (in 0.9% of the 227 samples), arsenic (7.0%) and uranium (19.4%) exceeded the values in WHO health-based guidelines for drinking-water quality. Maximum chromium, arsenic and uranium levels in the water samples were 1.3-, 10.4- and 17.2-fold higher than the values in the guidelines, respectively. We next focused on uranium, which is the most seriously polluted element among the 10 elements. Mean ± SD (138.0 ± 1.4) of the 238 U/ 235 U isotopic ratio in the water samples was in the range of previously reported ratios for natural source uranium. We then examined the effect of our originally developed magnesium (Mg)-iron (Fe)-based hydrotalcite-like compounds (MF-HT) on adsorption for uranium. All of the uranium-polluted well water samples from Kabul (mean ± SD = 190.4 ± 113.9 μg/L; n = 11) could be remediated up to 1.2 ± 1.7 μg/L by 1% weight of our MF-HT within 60 s at very low cost (<0.001 cents/day/family) in theory. Thus, we demonstrated not only elevated levels of some toxic elements including natural source uranium but also an effective depurative for uranium in well drinking water from Kabul. Since our depurative is effective for remediation of arsenic as shown in our previous studies, its practical use in Kabul may be encouraged. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

Incorporation of Uranium: II. Distribution of Uranium Absorbed through the Lungs and the Skin

PubMed Central

Walinder, G.; Fries, B.; Billaudelle, U.

1967-01-01

In experiments on mice, rabbits, and piglets the distribution of uranium was studied at different times after exposure. Uranium was administered by inhalation (mice) and through the skin (rabbits and piglets). These investigations show that the uptakes of uranium in different organs of the three species are highly dependent on the amounts administered. There seems to be a saturation effect in the spleen and bone tissue whenever the uranium concentration in the blood exceeds a certain level. The effect in the kidney is completely different. If, in a series of animals, the quantity of uranium is continuously increased, the uptakes by the kidneys increase more rapidly than the quantities administered. This observation seems to be consistent with the toxic effects of uranium on the capillary system in the renal cortex. Polyphloretin phosphate, a compound which reduces permeability, was investigated with respect to its effect on the uptake of uranium deposited in skin wounds in rabbits and piglets. It significantly reduced the absorption of uranium, even from depots in deep wounds. The findings are discussed with reference to the routine screening of persons exposed to uranium at AB Atomenergi. Images PMID:6073090

Multiconfigurational nature of 5f orbitals in uranium and plutonium intermetallics

PubMed Central

Booth, C.H.; Jiang, Yu; Wang, D.L.; Mitchell, J.N.; Tobash, P.H.; Bauer, E.D.; Wall, M.A.; Allen, P.G.; Sokaras, D.; Nordlund, D.; Weng, T.-C.; Torrez, M.A.; Sarrao, J.L.

2012-01-01

Uranium and plutonium’s 5f electrons are tenuously poised between strongly bonding with ligand spd-states and residing close to the nucleus. The unusual properties of these elements and their compounds (e.g., the six different allotropes of elemental plutonium) are widely believed to depend on the related attributes of f-orbital occupancy and delocalization for which a quantitative measure is lacking. By employing resonant X-ray emission spectroscopy (RXES) and X-ray absorption near-edge structure (XANES) spectroscopy and making comparisons to specific heat measurements, we demonstrate the presence of multiconfigurational f-orbital states in the actinide elements U and Pu and in a wide range of uranium and plutonium intermetallic compounds. These results provide a robust experimental basis for a new framework toward understanding the strongly-correlated behavior of actinide materials. PMID:22706643

Target materials for exotic ISOL beams

NASA Astrophysics Data System (ADS)

Gottberg, A.

2016-06-01

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

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

Reilly, Sean Douglas; Smith, Paul Herrick; Jarvinen, Gordon D.

Understanding the water solubility of plutonium and uranium compounds and residues at TA-55 is necessary to provide a technical basis for appropriate criticality safety, safety basis and accountability controls. Individual compound solubility was determined using published solubility data and solution thermodynamic modeling. Residue solubility was estimated using a combination of published technical reports and process knowledge of constituent compounds. The scope of materials considered includes all compounds and residues at TA-55 as of March 2016 that contain Pu-239 or U-235 where any single item in the facility has more than 500 g of nuclear material. This analysis indicates that themore » following materials are not appreciably soluble in water: plutonium dioxide (IDC=C21), plutonium phosphate (IDC=C66), plutonium tetrafluoride (IDC=C80), plutonium filter residue (IDC=R26), plutonium hydroxide precipitate (IDC=R41), plutonium DOR salt (IDC=R42), plutonium incinerator ash (IDC=R47), uranium carbide (IDC=C13), uranium dioxide (IDC=C21), U 3O 8 (IDC=C88), and uranium filter residue (IDC=R26). This analysis also indicates that the following materials are soluble in water: plutonium chloride (IDC=C19) and uranium nitrate (IDC=C52). Equilibrium calculations suggest that PuOCl is water soluble under certain conditions, but some plutonium processing reports indicate that it is insoluble when present in electrorefining residues (R65). Plutonium molten salt extraction residues (IDC=R83) contain significant quantities of PuCl 3, and are expected to be soluble in water. The solubility of the following plutonium residues is indeterminate due to conflicting reports, insufficient process knowledge or process-dependent composition: calcium salt (IDC=R09), electrorefining salt (IDC=R65), salt (IDC=R71), silica (IDC=R73) and sweepings/screenings (IDC=R78). Solution thermodynamic modeling also indicates that fire suppression water buffered with a commercially-available phosphate buffer would significantly reduce the solubility of PuCl 3 by the precipitation of PuPO 4.« less

PREPARATION OF URANIUM TRIOXIDE

DOEpatents

Buckingham, J.S.

1959-09-01

The production of uranium trioxide from aqueous solutions of uranyl nitrate is discussed. The uranium trioxide is produced by adding sulfur or a sulfur-containing compound, such as thiourea, sulfamic acid, sulfuric acid, and ammonium sulfate, to the uranyl solution in an amount of about 0.5% by weight of the uranyl nitrate hexahydrate, evaporating the solution to dryness, and calcining the dry residue. The trioxide obtained by this method furnished a dioxide with a considerably higher reactivity with hydrogen fluoride than a trioxide prepared without the sulfur additive.

Formation of Neogenic Ores on the Dump-Heaps of Old Uranium Mines and on the Mine-Head of Mines under Exploitation; FORMATION DE MINERAUX NEOGENES SUR LES HALDES D'ANCIENNES MINES D'URANIUM ET SUR LE CARREAU DES MINES EN EXPLOITATION

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

Chervet, J.

1960-01-01

The major degradations suffered by primary and secondary uranium ores under the weathering action of air and water are assessed. Pyritic ores were found to be the most vunerable. The interactions between pynite oxidation products and urantferous compounds often lead to the formation of neogentc ores. (C.J.G.)

222Rn emanation from uranium-glazed ceramics.

PubMed

Biagioni, R N; Sheets, R W

2001-02-01

Orange-red uranium-glazed dinnerware was found to emanate 222Rn to produce an average of less than 0.1 Bq 222Rn decay per piece, which should have no associated health risks. Comparison of 222Rn emanation to 226Ra in glazes (measured by alpha spectrometry) indicated inefficient emanation (<5%) of 222Rn, consistent with the low radon levels observed and with the presence of 222Rn progeny in glazes. These studies also showed that reagent grade uranium compounds may emanate measurable 222Rn.

WELDING PROCESS

DOEpatents

Zambrow, J.; Hausner, H.

1957-09-24

A method of joining metal parts for the preparation of relatively long, thin fuel element cores of uranium or alloys thereof for nuclear reactors is described. The process includes the steps of cleaning the surfaces to be jointed, placing the sunfaces together, and providing between and in contact with them, a layer of a compound in finely divided form that is decomposable to metal by heat. The fuel element members are then heated at the contact zone and maintained under pressure during the heating to decompose the compound to metal and sinter the members and reduced metal together producing a weld. The preferred class of decomposable compounds are the metal hydrides such as uranium hydride, which release hydrogen thus providing a reducing atmosphere in the vicinity of the welding operation.

Dibutyl Phosphoric Acid Solubility in High-Acid, Uranium-Bearing Solutions at SRS

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

Pierce, R.A.

1998-10-02

The Savannah River Site has enriched uranium (EU) solution which has been stored for almost 10 years since being purified in the second uranium cycle of the H area solvent extraction process. The concentrations in solution are approximately 6 g/L U and about 0.1 M nitric acid. Residual tributylphosphate in the solutions has slowly hydrolyzed to form dibutyl phosphoric acid (HDBP) at concentrations averaging 50 mg/L. Uranium is known to form compounds with the dibutylphosphate ion (DBP) which have limited solubility. The potential to form uranium-DBP solids raises a nuclear criticality safety issue. Prior SRTC tests (WSRC-TR-98-00188) showed that U-DBPmore » solids precipitate at concentrations potentially attainable during the storage of enriched uranium solutions. Furthermore, evaporation of the existing EUS solution without additional acidification could result in the precipitation of U-DBP solids if the DBP concentration in the resulting solution exceeds 110 mg/L at ambient temperature. The same potential exists for evaporation of unwashed 1CU solutions. As a follow-up to the earlier studies, SRTC studied the solubility limits for solutions containing acid concentrations above 0.5M HNO3. The data obtained in these tests reveals a shift to higher levels of DBP solubility above 0.5M HNO3 for both 6 g/L and 12 g/L uranium solutions. Analysis of U-DBP solids from the tests identified a mixture of different molecular structures for the solids created. The analysis distinguished UO2(DBP)2 as the dominant compound present at low acid concentrations. As the acid concentration increases, the crystalline UO2(DBP)2 shows molecular substitutions and an increase in amorphous content. Further analysis by methods not available at SRS will be needed to better identify the specific compounds present. This data indicates that acidification prior to evaporation can be used to increase the margin of safety for the storage of the EUS solutions. Subsequent experimentation evaluated options for absorbing HDBP from solution using either activated carbon or anion exchange resin. The activated carbon outperformed the anion exchange resin. Activated carbon absorbs DBP rapidly and has demonstrated the capability of absorbing 15 mg of DBP per gram of activated carbon. Analytical results also show that activated carbon absorbs uranium up to 17 mg per gram of carbon. It is speculated that the uranium absorbed is part of a soluble U-DBP complex that has been absorbed. Additional testing must still be performed to 1) establish absorption limits for uranium for anion exchange resin, 2) evaluate desorption characteristics of uranium and DBP, and 3) study the possibility of re-using the absorbent.« less

Preparative separation of phenolic compounds from Halimodendron halodendron by high-speed counter-current chromatography.

PubMed

Wang, Jihua; Gao, Haifeng; Zhao, Jianglin; Wang, Qi; Zhou, Ligang; Han, Jianguo; Yu, Zhu; Yang, Fuyu

2010-08-31

Three phenolic compounds, p-hydroxybenzoic acid (1), isorhamnetin-3-O-β-D-rutinoside (2), and 3,3'-di-O-methylquercetin (5), along with a phenolic mixture were successfully separated from the ethyl acetate crude extract of Halimodendron halodendron by high-speed counter-current chromatography (HSCCC) with chloroform-methanol-water-acetic acid (4:3:2:0.05, v/v) as the two-phase solvent system. The phenolic mixture from HSCCC was further separated by preparative HPLC and purified by Sephadex LH-20 to afford quercetin (3) and 3-O-methylquercetin (4). Seven hundred mg of ethyl acetate crude extract was separated by HSCCC to obtain six fractions which were then analyzed by high performance liquid chromatography (HPLC). The HSCCC separation obtained total of 80 mg of the mixture of quercetin (3) and 3-O-methylquercetin (4) (26.43% and 71.89%, respectively) in fraction 2, 14 mg of 3,3'-di-O-methylquercetin (5) at 95.14% of purity in fraction 3, 15 mg of p-hydroxybenzoic acid (1) at 92.83% of purity in fraction 5, 12 mg of isorhamnetin-3-O-β-D-rutinoside (2) at 97.99% of purity in fraction 6. This is the first time these phenolic compounds have been obtained from H. halodendron, and their chemical structures identified by means of physicochemical and spectrometric analysis.

Francis Perrin's 1939 Analysis of Uranium Criticality

NASA Astrophysics Data System (ADS)

Reed, Cameron

2012-03-01

In May 1939, French physicist Francis Perrin published the first numerical estimate of the fast-neutron critical mass of a uranium compound. While his estimate of about 40 metric tons (12 tons if tamped) pertained to uranium oxide of natural isotopic composition as opposed to the enriched uranium that would be required for a nuclear weapon, it is interesting to examine Perrin's physics and to explore the subsequent impact of his paper. In this presentation I will discuss Perrin's model, the likely provenance of his parameter values, and how his work compared to the approach taken by Robert Serber in his 1943 Los Alamos Primer.

Properties of radio-frequency heated argon confined uranium plasmas

NASA Technical Reports Server (NTRS)

1976-01-01

Pure uranium hexafluoride (UF6) was injected into an argon confined, steady state, rf-heated plasma within a fused silica peripheral wall test chamber. Exploratory tests conducted using an 80 kW rf facility and different test chamber flow configurations permitted selection of the configuration demonstrating the best confinement characteristics and minimum uranium compound wall coating. The overall test results demonstrated applicable flow schemes and associated diagnostic techniques were developed for the fluid mechanical confinement and characterization of uranium within an rf plasma discharge when pure UF6 is injected for long test times into an argon-confined, high-temperature, high-pressure, rf-heated plasma.

Reductive precipitation of metals photosensitized by tin and antimony porphyrins

DOEpatents

Shelnutt, John A.; Gong, Weiliang; Abdelouas, Abdesselam; Lutze, Werner

2003-09-30

A method for reducing metals using a tin or antimony porphyrin by forming an aqueous solution of a tin or antimony porphyrin, an electron donor, such as ethylenediaminetetraaceticacid, triethylamine, triethanolamine, and sodium nitrite, and at least one metal compound selected from a uranium-containing compound, a mercury-containing compound, a copper-containing compound, a lead-containing compound, a gold-containing compound, a silver-containing compound, and a platinum-containing compound through irradiating the aqueous solution with light.

Dry phase reactor for generating medical isotopes

DOEpatents

Mackie, Thomas Rockwell; Heltemes, Thad Alexander

2016-05-03

An apparatus for generating medical isotopes provides for the irradiation of dry-phase, granular uranium compounds which are then dissolved in a solvent for separation of the medical isotope from the irradiated compound. Once the medical isotope is removed, the dissolved compound may be reconstituted in dry granular form for repeated irradiation.

Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions

NASA Technical Reports Server (NTRS)

Wheeler, D. R.

1978-01-01

X-ray photoelectron spectroscopy was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

THE QUESTIONS OF HEALTH HAZARDS FROM THE INHALATION OF INSOLUBLE URANIUM AND THORIUM OXIDES

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

Hodge, H.C.; Thomas, R.G.

1958-10-31

The insoluble compounds of uranium and thorium, particularly the oxides, are important in the development of atomic energy. Thc questions of health hazards from exposures to dusts of these insoluble compounds are strikily simlar in many but not all respects, Among the similarities may be listed the following facts: The insoluble compounds present no chemical hazard. Both uranium and thorium dioxides, for example, are remarkably inert physiologically. No radiation injuries have so far been described in the lungs of experimental animals inhaling dust concentrations many times the recommended MAC. The lungs of a few dogs studied seven years after excessivemore » inhalation exposures to ThO/sub 2/ gave negative histological findings although high concentrations of thorium were present. The MACs for insoluble uranium and for inxoluble thorium dusts are identical, specifically 3 x 10/sup -11/ c/1. Calculated on a radiation basis, a lower MAC is appropriate for thorium. Based on a considerable body of information from cted. For both uranium and thorium dioxides fecal excretion reflects the immediate exposure to dusty atmospheres. Urine analyses are a prime index of uranium exposure whereas the presence of the much less soluble thorium dioxide in the lung cannot be thus assessed. Breath thoron extimnations or possibly measurements using a whole body counter have been recommended as indices of thorium exposure. The fundamental question depends on the radiosensitivity of the lung and of the pulmonary lymph nodes; neither the production of radiation injury nor the production of cancer are evaluated at present with respect to dosage of radiation. The lung tissues of the dogs described above must have received several thousand rem during the 7 year period. The pulmonary lymph modes must have received considerably more radiation because the concentrations in these nodes e use of the insoluble oxides and the low MACs combine to raise recurring questions of health hazards. (auth)« less

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

Fincke, J.R.; Swank, W.D.; Haggard, D.C.

This paper describes the experimental demonstration of a process for the direct plasma reduction of depleted uranium hexafluoride to uranium metal. The process exploits the large departures from equilibrium that can be achieved in the rapid supersonic expansion of a totally dissociated and partially ionized mixture of UF{sub 6}, Ar, He, and H{sub 2}. The process is based on the rapid condensation of subcooled uranium vapor and the relatively slow rate of back reaction between metallic uranium and HF to F{sub 2} to reform stable fluorides. The high translational velocities and rapid cooling result in an overpopulation of atomic hydrogenmore » which persists throughout the expansion process. Atomic hydrogen shifts the equilibrium composition by inhibiting the reformation of uranium-fluorine compounds. This process has the potential to reduce the cost of reducing UF{sub 6} to uranium metal with the added benefit of being a virtually waste free process. The dry HF produced is a commodity which has industrial value.« less

Plasmachemical synthesis and evaluation of the thermal conductivity of metal-oxide compounds "Molybdenum-uranium dioxide"

NASA Astrophysics Data System (ADS)

Kotelnikova, Alexandra A.; Karengin, Alexander G.; Mendoza, Orlando

2018-03-01

The article represents possibility to apply oxidative and reducing plasma for plasma-chemical synthesis of metal-oxide compounds «Mo‒UO2» from water-salt mixtures «molybdic acid‒uranyl nitrate» and «molybdic acid‒ uranyl acetate». The composition of water-salt mixture was calculated and the conditions ensuring plasma-chemical synthesis of «Mo‒UO2» compounds were determined. Calculations were carried out at atmospheric pressure over a wide range of temperatures (300-4000 K), with the use of various plasma coolants (air, hydrogen). The heat conductivity coefficients of metal-oxide compounds «Mo‒UO2» consisting of continuous component (molybdenum matrix) are calculated. Inclusions from ceramics in the form of uranium dioxide were ordered in the matrix. Particular attention is paid to methods for calculating the coefficients of thermal conductivity of these compounds with the use of different models. Calculated results were compared with the experimental data.

Laboratory-scale uranium RF plasma confinement experiments

NASA Technical Reports Server (NTRS)

Roman, W. C.

1976-01-01

An experimental investigation was conducted using 80 kW and 1.2 MW RF induction heater facilities to aid in developing the technology necessary for designing a self-critical fissioning uranium plasma core reactor. Pure uranium hexafluoride (UF6) was injected into argon-confined, steady-state, RF-heated plasmas in different uranium plasma confinement tests to investigate the characteristics of plamas core nuclear reactors. The objectives were: (1) to confine as high a density of uranium vapor as possible within the plasma while simultaneously minimizing the uranium compound wall deposition; (2) to develop and test materials and handling techniques suitable for use with high-temperature, high-pressure gaseous UF6; and (3) to develop complementary diagnostic instrumentation and measurement techniques to characterize the uranium plasma and residue deposited on the test chamber components. In all tests, the plasma was a fluid-mechanically-confined vortex-type contained within a fused-silica cylindrical test chamber. The test chamber peripheral wall was 5.7 cm ID by 10 cm long.

Economic analysis of crystal growth in space

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Chung, A. M.; Yan, C. S.; Mccreight, L. R.

1972-01-01

Many advanced electronic technologies and devices for the 1980's are based on sophisticated compound single crystals, i.e. ceramic oxides and compound semiconductors. Space processing of these electronic crystals with maximum perfection, purity, and size is suggested. No ecomonic or technical justification was found for the growth of silicon single crystals for solid state electronic devices in space.

Chemistry of peroxide compounds

NASA Technical Reports Server (NTRS)

Volnov, I. I.

1981-01-01

The history of Soviet research from 1866 to 1967 on peroxide compounds is reviewed. This research dealt mainly with peroxide kinetics, reactivity and characteristics, peroxide production processes, and more recently with superoxides and ozonides and emphasis on the higher oxides of group 1 and 2 elements. Solid state fluidized bed synthesis and production of high purity products based on the relative solubilities of the initial, intermediate, and final compounds and elements in liquid ammonia are discussed.

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

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

DOE PAGES

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso; ...

2017-02-02

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

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

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Characteristics of uranium carbonitride microparticles synthesized using different reaction conditions

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

Silva, Chinthaka M; Lindemer, Terrence; Voit, Stewart L

2014-11-01

Three sets of different experimental conditions by changing the cover gases during the sample preparation were tested to synthesize uranium carbonitride (UC1-xNx) microparticles. In the first two sets of experiments using (N2 to N2-4%H2 to Ar) and (Ar to N2 to Ar) environments, single phase UC1-xNx was synthesized. When reducing environments (Ar-4%H2 to N2-4%H2 to Ar-4%H2) were utilized, theoretical densities up to 97% of single phase UC1-xNx kernels were obtained. Physical and chemical characteristics such as density, phase purity, and chemical compositions of the synthesized UC1-xNx materials for the diferent experimental conditions used are provided. In-depth analysis of the microstruturesmore » of UC1-xNx has been carried out and is discussed with the objective of large batch fabrication of high density UC1-xNx kernels.« less

Hybrid Interferometric/Dispersive Atomic Spectroscopy For Nuclear Materials Analysis

NASA Astrophysics Data System (ADS)

Morgan, Phyllis K.

Laser-induced breakdown spectroscopy (LIBS) is an optical emission spectroscopy technique that holds promise for detection and rapid analysis of elements relevant for nuclear safeguards and nonproliferation, including the measurement of isotope ratios. One important application of LIBS is the measurement of uranium enrichment (235U/238U), which requires high spectral resolution (e.g., 25 pm for the 424.437 nm U II line). Measuring uranium enrichment is important in nuclear nonproliferation and safeguards because the uranium highly enriched in the 235U isotope can be used to construct nuclear weapons. High-resolution dispersive spectrometers necessary for such measurements are typically bulky and expensive. A hybrid interferometric/dispersive spectrometer prototype, which consists of an inexpensive, compact Fabry-Perot etalon integrated with a low to moderate resolution Czerny-Turner spectrometer, was assembled for making high-resolution measurements of nuclear materials in a laboratory setting. To more fully take advantage of this low-cost, compact hybrid spectrometer, a mathematical reconstruction technique was developed to accurately reconstruct relative line strengths from complex spectral patterns with high resolution. Measurement of the mercury 313.1555/313.1844 nm doublet from a mercury-argon lamp yielded a spectral line intensity ratio of 0.682, which agrees well with an independent measurement by an echelle spectrometer and previously reported values. The hybrid instrument was used in LIBS measurements and achieved the resolution needed for isotopic selectivity of LIBS of uranium in ambient air. The samples used were a natural uranium foil (0.7% of 235U) and a uranium foil highly enriched in 235U to 93%. Both samples were provided by the Penn State University's Breazeale Nuclear Reactor. The enrichment of the uranium foils was verified using a high-purity germanium detector and dedicated software for multi-group spectral analysis. Uranium spectral line widths of ˜10 pm were measured at a center wavelength 424.437 nm, clearly discriminating the natural from the highly enriched uranium at that wavelength. The 424.167 nm isotope shift (˜6 pm), limited by spectral broadening, was only partially resolved but still discernible. This instrument and reconstruction method could enable the design of significantly smaller, portable high-resolution instruments with isotopic specificity, benefiting nuclear safeguards, treaty verification, nuclear forensics, and a variety of other spectroscopic applications.

Implementation of ICP-MS protocols for uranium urinary measurements in worker monitoring.

PubMed

Baglan, N; Cossonnet, C; Trompier, F; Ritt, J; Bérard, P

1999-10-01

The uranium concentration in human urine spiked with natural uranium and rat urine containing metabolized depleted uranium was determined by ICP-MS. The use of ICP-MS was investigated without any chemical treatment or after the different stages of a purification protocol currently carried out for routine monitoring. In the case of spiked urine, the measured uranium concentrations were consistent with those certified by an intercomparison network in radiotoxicological analysis (PROCORAD) and with those obtained by alpha spectrometry in the case of the urine containing metabolized uranium. The quantitative information which could be obtained in the different protocols investigated shows the extent to which ICP-MS provides greater flexibility for setting up appropriate monitoring approaches in radiation protection routines and accidental situations. This is due to the combination of high sensitivity and the accuracy with which traces of uranium in urine can be determined in a shorter time period. Moreover, it has been shown that ICP-MS measurement can be used to quantify the 235U isotope, which is useful for characterizing the nature of the uranium compound, but difficult to perform using alpha spectrometry.

Use of an ion mobility spectrometer for detecting uranium compounds

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

McLain, Derek R.; Steeb, Jennifer L.; Smith, Nicholas A.

The safeguards community currently lacks a method to rapidly determine the chemical form of radioactive and non-radioactive compounds in real time during inspection activities. Chemical speciation identification can provide important information on both the types of materials that are collected during environmental sampling and can inform inspectors as to where to focus efforts during inspections or complementary access visits. Ion Mobility Spectrometry (IMS) is an established field technique for the detection of explosives, narcotics, and other organic compounds. More recently, electrospray ionization (ESI) has been used to introduce inorganic compounds to IMS instruments for analysis. These techniques have shown themore » ability to supply chemical information about the compounds being analyzed. Although these laboratory based instruments use a liquid-based injection system, there is evidence in the literature of unaltered and intact pharmaceutical tablets being volatilized and ionized in open atmosphere using heat and a Ni-63 source. Lastly, this work determined that a commercial-off-the-shelf (COTS) IMS could be used for the identification of solid uranium compounds directly after sampling using a COTS sample swipe.« less

Use of an ion mobility spectrometer for detecting uranium compounds

DOE PAGES

McLain, Derek R.; Steeb, Jennifer L.; Smith, Nicholas A.

2018-03-09

The safeguards community currently lacks a method to rapidly determine the chemical form of radioactive and non-radioactive compounds in real time during inspection activities. Chemical speciation identification can provide important information on both the types of materials that are collected during environmental sampling and can inform inspectors as to where to focus efforts during inspections or complementary access visits. Ion Mobility Spectrometry (IMS) is an established field technique for the detection of explosives, narcotics, and other organic compounds. More recently, electrospray ionization (ESI) has been used to introduce inorganic compounds to IMS instruments for analysis. These techniques have shown themore » ability to supply chemical information about the compounds being analyzed. Although these laboratory based instruments use a liquid-based injection system, there is evidence in the literature of unaltered and intact pharmaceutical tablets being volatilized and ionized in open atmosphere using heat and a Ni-63 source. Lastly, this work determined that a commercial-off-the-shelf (COTS) IMS could be used for the identification of solid uranium compounds directly after sampling using a COTS sample swipe.« less

COORDINATION COMPOUND-SOLVENT EXTRACTION PROCESS FOR URANIUM RECOVERY

DOEpatents

Reas, W.H.

1959-03-10

A method is presented for the separation of uranium from aqueous solutions containing a uranyl salt and thorium. Thc separation is effected by adding to such solutions an organic complexing agent, and then contacting the solution with an organic solvent in which the organic complexing agent is soluble. By use of the proper complexing agent in the proper concentrations uranium will be complexed and subsequently removed in the organic solvent phase, while the thorium remains in the aqueous phase. Mentioned as suitable organic complexing agents are antipyrine, bromoantipyrine, and pyramidon.

Thermodynamic properties of selected uranium compounds and aqueous species at 298.15 K and 1 bar and at higher temperatures; preliminary models for the origin of coffinite deposits

USGS Publications Warehouse

Hemingway, B.S.

1982-01-01

Thermodynamic values for 110 uranium-bearing phases and 28 aqueous uranium solution species (298.15 K and l bar) are tabulated based upon evaluated experimental data (largely from calorimetric experiments) and estimated values. Molar volume data are given for most of the solid phases. Thermodynamic values for 16 uranium-bearing phases are presented for higher temperatures in the form of and as a supplement to U.S. Geological Survey Bulletin 1452 (Robie et al., 1979). The internal consistency of the thermodynamic values reported herein is dependent upon the reliability of the experimental results for several uranium phases that have been used as secondary calorimetric reference phases. The data for the reference phases and for those phases evaluated with respect to the secondary reference phases are discussed. A preliminary model for coffinite formation has been proposed together with an estimate of the free energy of formation of coffinite. Free energy values are estimated for several other uranium-bearing silicate phases that have been reported as secondary uranium phases associated with uranium ore deposits and that could be expected to develop wherever uranium is leached by groundwaters.

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.

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

PubMed

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

2015-03-13

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

Syntheses, Characterization, Resolution, and Biological Studies of Coordination Compounds of Aspartic Acid and Glycine

PubMed Central

Akinkunmi, Ezekiel; Ojo, Isaac; Adebajo, Clement; Isabirye, David

2017-01-01

Enantiomerically enriched coordination compounds of aspartic acid and racemic mixtures of coordination compounds of glycine metal-ligand ratio 1 : 3 were synthesized and characterized using infrared and UV-Vis spectrophotometric techniques and magnetic susceptibility measurements. Five of the complexes were resolved using (+)-cis-dichlorobis(ethylenediamine)cobalt(III) chloride, (+)-bis(glycinato)(1,10-phenanthroline)cobalt(III) chloride, and (+)-tris(1,10-phenanthroline)nickel(II) chloride as resolving agents. The antimicrobial and cytotoxic activities of these complexes were then determined. The results obtained indicated that aspartic acid and glycine coordinated in a bidentate fashion. The enantiomeric purity of the compounds was in the range of 22.10–32.10%, with (+)-cis-dichlorobis(ethylenediamine)cobalt(III) complex as the more efficient resolving agent. The resolved complexes exhibited better activity in some cases compared to the parent complexes for both biological activities. It was therefore inferred that although the increase in the lipophilicity of the complexes may assist in the permeability of the complexes through the cell membrane of the pathogens, the enantiomeric purity of the complexes is also of importance in their activity as antimicrobial and cytotoxic agents. PMID:28293149

Thermodynamic Simulation of Equilibrium Composition of Reaction Products at Dehydration of a Technological Channel in a Uranium-Graphite Reactor

NASA Astrophysics Data System (ADS)

Pavliuk, A. O.; Zagumennov, V. S.; Kotlyarevskiy, S. G.; Bespala, E. V.

2018-01-01

The problems of accumulation of nuclear fuel spills in the graphite stack in the course of operation of uranium-graphite nuclear reactors are considered. The results of thermodynamic analysis of the processes in the graphite stack at dehydration of a technological channel, fuel element shell unsealing and migration of fission products, and activation of stable nuclides in structural elements of the reactor and actinides inside the graphite moderator are given. The main chemical reactions and compounds that are produced in these modes in the reactor channel during its operation and that may be hazardous after its shutdown and decommissioning are presented. Thermodynamic simulation of the equilibrium composition is performed using the specialized code TERRA. The results of thermodynamic simulation of the equilibrium composition in different cases of technological channel dehydration in the course of the reactor operation show that, if the temperature inside the active core of the nuclear reactor increases to the melting temperature of the fuel element, oxides and carbides of nuclear fuel are produced. The mathematical model of the nonstationary heat transfer in a graphite stack of a uranium-graphite reactor in the case of the technological channel dehydration is presented. The results of calculated temperature evolution at the center of the fuel element, the replaceable graphite element, the air gap, and in the surface layer of the block graphite are given. The numerical results show that, in the case of dehydration of the technological channel in the uranium-graphite reactor with metallic uranium, the main reaction product is uranium dioxide UO2 in the condensed phase. Low probability of production of pyrophoric uranium compounds (UH3) in the graphite stack is proven, which allows one to disassemble the graphite stack without the risk of spontaneous graphite ignition in the course of decommissioning of the uranium-graphite nuclear reactor.

Direct vapor/solid synthesis of mercuric iodide using compounds of mercury and iodine

DOEpatents

Skinner, Nathan L.

1990-01-01

A process is disclosed for producing high purity mercuric iodide by passing a gaseous source of a mercuric compound through a particulate bed of a low vapor pressure iodide compound which is maintained at an elevated temperature which is the lower of either: (a) just below the melting or volatilization temperature of the iodide compound (which ever is lower); or (b) just below the volatilization point of the other reaction product formed during the reaction; to cause the mercuric compound to react with the iodide compound to form mercuric iodide which then passes as a vapor out of the bed into a cooler condensation region.

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

PubMed Central

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

2016-01-01

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

Vector representation as a tool for detecting characteristic uranium peaks

NASA Astrophysics Data System (ADS)

Forney, Anne Marie

Vector representation is found as a viable tool for identifying the presence of and determining the difference between enriched and naturally occurring uranium. This was accomplished through the isolation of two regions of interest around the uranium-235 (235U) gamma emission at 186 keV and the uranium-238 (238U) gamma emission at 1001 keV. The uranium 186 keV peak is used as a meter for uranium enrichment, and events from this emission occurred more frequently with the increase of the 235U composition. Spectra were taken with the use of a high purity germanium detector in series with a multi-channel analyzer (MCA) and Maestro 32, a MCA emulator and spectral software. The vector representation method was used to compare two spectra by taking their dot product. The output from this method is an angle, which represents the similarity and contrast between the two spectra. When the angle is close to zero the spectra are similar, and as the angle approaches 90 degrees the spectral agreement decreases. The angles were calculated and compared in Microsoft Excel. A 49 % enriched uranyl acetate source containing both gamma emissions from 235U and 238U was used as a reference source to which all spectra were compared. Two other uranium sources were used within this project: a 100.2 nCi highly-enriched uranium source with 97.7 % 235U by weight, and a piece of uranium ore with an approximate exposure rate of 0.2 mR/h (51.5 nC/kg/h) at 1 cm. These two uranium sources provided different ratios of 235U to 238U, leading to different ratios of the 186 keV and 1001 keV peaks. To test the limits of the vector representation method, various source configurations were used. These included placing the source directly on top of the detector, using two distances for the source from the detector, using the source in addition to cobalt-60, and finally two distances for the source from the detector with a one centimeter lead shield. The two distances from the detector without the shielding were 1.3 inches (3.30 cm) and 1 foot (30.48 cm). In the cases using lead shielding, in the first geometry, the source was placed directly on the lead shielding and in the second geometry, the source was placed a foot above the lead shielding and detector. Vector representation output angles higher than a value of 40.3 degrees indicated that uranium was not present in the source. All of the sources tested with an angle below this 40.3 degree cutoff contained some type of uranium. To determine whether the uranium was processed or naturally occurring, 18.0 degrees was chosen as the upper limit for processed uranium sources. Sources that produced an angle above 18.0 degrees and below 40.3 degrees were categorized as naturally occurring uranium. The vector representation technique was able to classify the uranium sources in all of the geometries except for the geometries that included the centimeter of lead.

21 CFR 184.1298 - Ferric citrate.

Code of Federal Regulations, 2014 CFR

2014-04-01

... prepared from reaction of citric acid with ferric hydroxide. It is a compound of indefinite ratio of citric acid and iron. (b) The ingredient must be of a purity suitable for its intended use. (c) In accordance...

Modeling of point defects and rare gas incorporation in uranium mono-carbide

NASA Astrophysics Data System (ADS)

Chartier, A.; Van Brutzel, L.

2007-02-01

An embedded atom method (EAM) potential has been established for uranium mono-carbide. This EAM potential was fitted on structural properties of metallic uranium and uranium mono-carbide. The formation energies of point defects, as well as activation energies for self migration, have been evaluated in order to cross-check the suitability of the potential. Assuming that the carbon vacancies are the main defects in uranium mono-carbide compounds, the migration paths and energies are consistent with experimental data selected by Catlow[C.R.A. Catlow, J. Nucl. Mater. 60 (1976) 151]. The insertion and migration energies for He, Kr and Xe have also been evaluated with available inter-atomic potentials [H.H. Andersen, P. Sigmund, Nucl. Instr. and Meth. B 38 (1965) 238]. Results show that the most stable defect configuration for rare gases is within uranium vacancies. The migration energy of an interstitial Xe is 0.5 eV, in agreement with the experimental value of 0.5 eV [Hj. Matzke, Science of advanced LMFBR fuels, Solid State Physics, Chemistry and Technology of Carbides, Nitrides and Carbonitrides of Uranium and Plutonium, North-Holland, 1986].

Thermodynamic properties of uranium in liquid gallium, indium and their alloys

NASA Astrophysics Data System (ADS)

Volkovich, V. A.; Maltsev, D. S.; Yamshchikov, L. F.; Osipenko, A. G.

2015-09-01

Activity, activity coefficients and solubility of uranium was determined in gallium, indium and gallium-indium alloys containing 21.8 (eutectic), 40 and 70 wt.% In. Activity was measured at 573-1073 K employing the electromotive force method, and solubility between room temperature (or the alloy melting point) and 1073 K employing direct physical measurements. Activity coefficients were obtained from the difference of experimentally determined temperature dependencies of uranium activity and solubility. Intermetallic compounds formed in the respective alloys were characterized using X-ray diffraction. Partial and excess thermodynamic functions of uranium in the studied alloys were calculated. Liquidus lines in U-Ga and U-In phase diagrams from the side rich in gallium or indium are proposed.

Uniform deposition of uranium hexafluoride (UF6): Standardized mass deposits and controlled isotopic ratios using a thermal fluorination method

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

McNamara, Bruce K.; O’Hara, Matthew J.; Casella, Andrew M.

2016-07-01

Abstract: We report a convenient method for the generation of volatile uranium hexafluoride (UF6) from solid uranium oxides and other uranium compounds, followed by uniform deposition of low levels of UF6 onto sampling coupons. Under laminar flow conditions, UF6 is shown to interact with surfaces within the chamber to a highly predictable degree. We demonstrate the preparation of uranium deposits that range between ~0.01 and 470±34 ng∙cm-2. The data suggest the method can be extended to creating depositions at the sub-picogram∙cm-2 level. Additionally, the isotopic composition of the deposits can be customized by selection of the uranium source materials. Wemore » demonstrate a layering technique whereby two uranium solids, each with a different isotopic composition, are employed to form successive layers of UF6 on a surface. The result is an ultra-thin deposit of UF6 that bears an isotopic signature that is a composite of the two uranium sources. The reported deposition method has direct application to the development of unique analytical standards for nuclear safeguards and forensics.« less

Safeguards Options for Natural Uranium Conversion Facilities ? A Collaborative Effort between the U.S. Department of Energy (DOE) and the National Nuclear Energy Commission of Brazil (CNEN)

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

Raffo-Caiado, Ana Claudia; Begovich, John M; Ferrada, Juan J

2008-01-01

In 2005, the National Nuclear Energy Commission of Brazil (CNEN) and the U.S. Department of Energy (DOE) agreed on a collaborative effort to evaluate measures that can strengthen the effectiveness of international safeguards at a natural uranium conversion plant (NUCP). The work was performed by DOE's Oak Ridge National Laboratory and CNEN. A generic model of an NUCP was developed and typical processing steps were defined. The study, completed in early 2007, identified potential safeguards measures and evaluated their effectiveness and impacts on operations. In addition, advanced instrumentation and techniques for verification purposes were identified and investigated. The scope ofmore » the work was framed by the International Atomic Energy Agency's (IAEA's) 2003 revised policy concerning the starting point of safeguards at uranium conversion facilities. Before this policy, only the final products of the uranium conversion plant were considered to be of composition and purity suitable for use in the nuclear fuel cycle and, therefore, subject to AEA safeguards control. DOE and CNEN have explored options for implementing the IAEA policy, although Brazil understands that the new policy established by the IAEA is beyond the framework of the Quadripartite Agreement of which it is one of the parties, together with Argentina, the Brazilian-Argentine Agency for Accounting and Control of Nuclear Materials, and the IAEA. This paper highlights the findings of this joint collaborative effort and identifies technical measures to strengthen international safeguards in NUCPs.« less

Separation of Protactinium Employing Sulfur-Based Extraction Chromatographic Resins.

PubMed

Mastren, Tara; Stein, Benjamin W; Parker, T Gannon; Radchenko, Valery; Copping, Roy; Owens, Allison; Wyant, Lance E; Brugh, Mark; Kozimor, Stosh A; Nortier, F Meiring; Birnbaum, Eva R; John, Kevin D; Fassbender, Michael E

2018-06-05

Protactinium-230 ( t 1/2 = 17.4 d) is the parent isotope of 230 U ( t 1/2 = 20.8 d), a radionuclide of interest for targeted alpha therapy (TAT). Column chromatographic methods have been developed to separate no-carrier-added 230 Pa from proton irradiated thorium targets and accompanying fission products. Results reported within demonstrate the use of novel sulfur bearing chromatographic extraction resins for the selective separation of protactinium. The recovery yield of 230 Pa was 93 ± 4% employing a R 3 P═S type commercially available resin and 88 ± 4% employing a DGTA (diglycothioamide) containing custom synthesized extraction chromatographic resin. The radiochemical purity of the recovered 230 Pa was measured via high purity germanium γ-ray spectroscopy to be >99.5% with the remaining radioactive contaminant being 95 Nb due to its similar chemistry to protactinium. Measured equilibrium distribution coefficients for protactinium, thorium, uranium, niobium, radium, and actinium on both the R 3 P═S type and the DGTA resin in hydrochloric acid media are reported, to the best of our knowledge, for the first time.

Plasma core reactor simulations using RF uranium seeded argon discharges

NASA Technical Reports Server (NTRS)

Roman, W. C.

1975-01-01

An experimental investigation was conducted using the United Technologies Research Center (UTRC) 80 kW and 1.2 MW RF induction heater systems to aid in developing the technology necessary for designing a self-critical fissioning uranium plasma core reactor (PCR). A nonfissioning, steady-state RF-heated argon plasma seeded with pure uranium hexafluoride (UF6) was used. An overall objective was to achieve maximum confinement of uranium vapor within the plasma while simultaneously minimizing the uranium compound wall deposition. Exploratory tests were conducted using the 80 kW RF induction heater with the test chamber at approximately atmospheric pressure and discharge power levels on the order of 10 kW. Four different test chamber flow configurations were tested to permit selection of the configuration offering the best confinement characteristics for subsequent tests at higher pressure and power in the 1.2 MW RF induction heater facility.

Parallel solution-phase synthesis of a 2-aminothiazole library including fully automated work-up.

PubMed

Buchstaller, Hans-Peter; Anlauf, Uwe

2011-02-01

A straightforward and effective procedure for the solution phase preparation of a 2-aminothiazole combinatorial library is described. Reaction, work-up and isolation of the title compounds as free bases was accomplished in a fully automated fashion using the Chemspeed ASW 2000 automated synthesizer. The compounds were obtained in good yields and excellent purities without any further purification procedure.

Metal alkoxides and methods of making same

DOEpatents

Hentges, Patrick J.; Greene, Laura H.; Pafford, Margaret Mary; Westwood, Glenn; Klemperer, Walter G.

2005-01-04

A method of making a superconducting structure includes depositing a metal alkoxide on a surface of a metal and hydrolyzing the metal alkoxide on the surface to form a pinhole-free film. The metal is a superconductor. The metal alkoxide may be a compound of formula (I): where M is zirconium or hafnium, and the purity of the compound is at least 97% as measured by NMR spectroscopy.

Evaluation of occupational exposure to naturally occurring radioactive materials in the Iranian ceramics industry.

PubMed

Fathabadi, N; Farahani, M V; Amani, S; Moradi, M; Haddadi, B

2011-06-01

Zircon contains small amounts of uranium, thorium and radium in its crystalline structure. The ceramic industry is one of the major consumers of zirconium compounds that are used as an ingredient at ∼10-20 % by weight in glaze. In this study, seven different ceramic factories have been investigated regarding the presence of radioactive elements with focus on natural radioactivity. The overall objective of this investigation is to provide information regarding the radiation exposure to workers in the ceramic industry due to naturally occurring radioactive materials. This objective is met by collecting existing radiological data specific to glaze production and generating new data from sampling activities. The sampling effort involves the whole process of glaze production. External exposures are monitored using a portable gamma-ray spectrometer and environmental thermoluminescence dosimeters, by placing them for 6 months in some workplaces. Internal routes of exposure (mainly inhalation) are studied using air sampling, and gross alpha and beta counting. Measurement of radon gas and its progeny is performed by continuous radon gas monitors that use pulse ionisation chambers. Natural radioactivity due to the presence of ²³⁸U, ²³²Th and ⁴⁰K in zirconium compounds, glazes and other samples is measured by a gamma-ray spectrometry system with a high-purity germanium detector. The average concentrations of ²³⁸U and ²³²Th observed in the zirconium compounds are >3300 and >550 Bq kg⁻¹, respectively. The specific activities of other samples are much lower than in zirconium compounds. The annual effective dose from external radiation had a mean value of ∼0.13 mSv y⁻¹. Dust sampling revealed the greatest values in the process at the powdering site and hand weighing places. In these plants, the annual average effective dose from inhalation of long-lived airborne radionuclides was 0.226 mSv. ²²²Rn gas concentrations in the glaze production plant and storage warehouse were found to range from 10 to 213 Bq m⁻³. In this study, the estimated annual effective doses to exposed workers were <1 mSv y⁻¹.

Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

PubMed

Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

2016-02-01

A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

Uranium-bearing lignite in southwestern North Dakota

USGS Publications Warehouse

Moore, George W.; Melin, Robert E.; Kepferle, Roy C.

1954-01-01

Uranium-bearing lignite was mapped and sampled in the Bullion Butte, Sentinel Butte, HT Butte, and Chalky Buttes areas in southwestern North Dakota. The uraniferous lignite occurs at several stratigraphic positions in the Sentinel Butte member of the Fort Union formation of Paleocene age. A total of 261 samples were collected for uranium analysis from 85 localities, Lignite contained as much as 0.045 percent uranium, 10.0 percent ash, and 0.45 percent uranium in the ash was found although the average is lower. Inferred reserves for the four areas examined are estimated to be about 27 million tons of lignite in beds about 2 feet thick and containing more than 3000 tons of uranium. The lignite in beds about 2 feet thick and containing more than 3000 tons of uranium. The lignite averages more than 30 percent ash in the surface samples. The principal factor that seems to influence the uranium content of lignite beds is their stratigraphic position below the overlying rocks of the White River group of Oligocene age. All of the uranium-bearing beds closely underlie the base of the White River group. Although this relationship seems to be the controlling factor, the relative concentration of uranium may be modified by other conditions. Beds enclosed in permeable rocks are more uraniferous than beds in impermeable rocks, and thin beds have higher content of uranium than thick beds. In addition, thick lignite beds commonly have a top=preferential distribution of uranium. These and other factors suggest that the uranium is secondary and this it was introduced by ground water which had leached uranium from volcanic ash in the overlying rocks of the White River group. It is thought that the uranium is held in the lignite as part of a metallo-organic compound.

21 CFR 184.1298 - Ferric citrate.

Code of Federal Regulations, 2011 CFR

2011-04-01

... Reg. No. 2338-05-8) is prepared from reaction of citric acid with ferric hydroxide. It is a compound of indefinite ratio of citric acid and iron. (b) The ingredient must be of a purity suitable for its...

21 CFR 184.1298 - Ferric citrate.

Code of Federal Regulations, 2012 CFR

2012-04-01

... Reg. No. 2338-05-8) is prepared from reaction of citric acid with ferric hydroxide. It is a compound of indefinite ratio of citric acid and iron. (b) The ingredient must be of a purity suitable for its...

21 CFR 184.1298 - Ferric citrate.

Code of Federal Regulations, 2010 CFR

2010-04-01

... Reg. No. 2338-05-8) is prepared from reaction of citric acid with ferric hydroxide. It is a compound of indefinite ratio of citric acid and iron. (b) The ingredient must be of a purity suitable for its...

21 CFR 184.1298 - Ferric citrate.

Code of Federal Regulations, 2013 CFR

2013-04-01

... Reg. No. 2338-05-8) is prepared from reaction of citric acid with ferric hydroxide. It is a compound of indefinite ratio of citric acid and iron. (b) The ingredient must be of a purity suitable for its...

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.

Electronic structure and fine structural features of the air-grown UNxOy on nitrogen-rich uranium nitride

NASA Astrophysics Data System (ADS)

Long, Zhong; Zeng, Rongguang; Hu, Yin; Liu, Jing; Wang, Wenyuan; Zhao, Yawen; Luo, Zhipeng; Bai, Bin; Wang, Xiaofang; Liu, Kezhao

2018-06-01

Oxide formation on surface of nitrogen-rich uranium nitride film/particles was investigated using X-ray photoelectron spectroscopy (XPS), auger electron spectroscopy (AES), aberration-corrected transmission electron microscopy (TEM), and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) coupled with electron energy-loss spectroscopy (EELS). XPS and AES studies indicated that the oxidized layer on UN2-x film is ternary compound uranium oxynitride (UNxOy) in 5-10 nm thickness. TEM/HAADF-STEM and EELS studies revealed the UNxOy crystallizes in the FCC CaF2-type structure with the lattice parameter close to the CaF2-type UN2-x matrix. The work can provide further information to the oxidation mechanism of uranium nitride.

Implications of modelled radioactivity measurements along coastal Odisha, Eastern India for heavy mineral resources

NASA Astrophysics Data System (ADS)

Ghosal, S.; Agrahari, S.; Guin, R.; Sengupta, D.

2017-01-01

A radioelemental assemblage assessment of two beaches of Odisha is performed for the first time. The radiation is measured in two ways, both on field with the help of a hand held environmental survey meter and in the laboratory, where the concentrations of radionuclide's 238U, 232Th and 4K have been determined with the help of High Purity Germanium detector (HPGe). Mineralogical analysis of selected samples has been performed with the help of X-Ray Fluorescence Spectrometry (XRF). A marked difference between the concentration of Uranium (274 Bq kg-1) and Thorium (2489 Bq kg-1) is observed and discussed based on the geology of the area. The placer deposits showing an enrichment of thorium can be an important source of nuclear fuel for the thorium based nuclear reactors. The ratio of thorium and uranium concentrations gives us an idea about the coastal processes associated with the beach. Statistical analysis of the data shows a positive correlation between 238U and 232Th and a strong negative correlation is indicated between 4 K and 238U, 232Th. A cross plot between the equivalent thorium and the equivalent uranium and the equivalent thorium and potassium, represents the nature of deposition and its association with the heavy mineral along with the radioactive elements. Heavy minerals exhibit an increasing trend towards Northeast-Southwest along the south eastern coast of India.

Solubility limits of dibutyl phosphoric acid in uranium-nitric acid solutions

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

Pierce, R.A.

2000-01-04

The Savannah River Site has enriched uranium (EU) solution that has been stored since being purified in its solvent extraction processes. The concentrations in solution are approximately 6 g/L U and 0.1 M nitric acid. Residual tributylphosphate in solution has slowly hydrolyzed to form dibutyl phosphoric acid (HDBP) at concentrations averaging 30--50 mg/L. Dibutyl phosphoric acid, in turn, is in equilibrium with (HDBP){sub 2} and DBP{sup {minus}}. Uranium can form compounds with the dibutylphosphate ion (DBP{sup {minus}}) which have limited solubility, thereby creating a nuclear criticality safety issue. Literature reports and earlier SRTC tests have shown that it is feasiblemore » to precipitate U-DBP solid during the storage and processing of EU solutions. As a result, a series of solubility experiments were run at nitric acid concentrations from 0--4.0 M HNO{sub 3}, uranium at 0--90 g/L, and temperatures from 0--30 C. The data shows temperature and nitric acid concentration dependence consistent with what would be expected. With respect to uranium concentration, U-DBP solubility passes through a minimum between 6 and 12 g/L U at the acid concentrations and temperatures studied. However, the minimum shows a slight shift toward lower uranium concentrations at lower nitric acid concentrations. The shifts in solubility are strongly dependent upon the overall ionic strength of the solution. The data also reveal a shift to higher DBP solubility above 0.5 M HNO{sub 3} for both 6 g/L and 12 g/L uranium solutions. Analysis of U-DBP solids from the tests identified distinct differences between precipitates from less than 0.5 M solutions and those from greater than 4 M acid. Analyses identified UO{sub 2}(DBP){sub 2} as the dominant compound present at low acid concentrations in accordance with literature reports. As the acid concentration increases, the crystalline UO{sub 2}(DBP){sub 2} shows molecular substitutions and an increase in amorphous content.« less

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.

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.

Vapor Pressure Data and Analysis for Selected HD Decomposition Products: 1,4-Thioxane, Divinyl Sulfoxide, Chloroethyl Acetylsulfide, and 1,4-Dithiane

DTIC Science & Technology

2018-06-01

decomposition products from bis-(2-chloroethyl) sulfide (HD). These data were measured using an ASTM International method that is based on differential...2.1 Materials and Method ........................................................................................2 2.2 Data Analysis...and Method The source and purity of the materials studied are listed in Table 1. Table 1. Sample Information for Title Compounds Compound

A high-resolution peak fractionation approach for streamlined screening of nuclear-factor-E2-related factor-2 activators in Salvia miltiorrhiza.

PubMed

Zhang, Hui; Luo, Li-Ping; Song, Hui-Peng; Hao, Hai-Ping; Zhou, Ping; Qi, Lian-Wen; Li, Ping; Chen, Jun

2014-01-24

Generation of a high-purity fraction library for efficiently screening active compounds from natural products is challenging because of their chemical diversity and complex matrices. In this work, a strategy combining high-resolution peak fractionation (HRPF) with a cell-based assay was proposed for target screening of bioactive constituents from natural products. In this approach, peak fractionation was conducted under chromatographic conditions optimized for high-resolution separation of the natural product extract. The HRPF approach was automatically performed according to the predefinition of certain peaks based on their retention times from a reference chromatographic profile. The corresponding HRPF database was collected with a parallel mass spectrometer to ensure purity and characterize the structures of compounds in the various fractions. Using this approach, a set of 75 peak fractions on the microgram scale was generated from 4mg of the extract of Salvia miltiorrhiza. After screening by an ARE-luciferase reporter gene assay, 20 diterpene quinones were selected and identified, and 16 of these compounds were reported to possess novel Nrf2 activation activity. Compared with conventional fixed-time interval fractionation, the HRPF approach could significantly improve the efficiency of bioactive compound discovery and facilitate the uncovering of minor active components. Copyright © 2013 Elsevier B.V. All rights reserved.

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

Marshall, Margaret A.

In the early 1970s Dr. John T. Mihalczo (team leader), J.J. Lynn, and J.R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) in an effort to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950s. The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared with themore » GODIVA I experiments. Additionally, various material reactivity worths, the surface material worth coefficient, the delayed neutron fraction, the prompt neutron decay constant, relative fission density, and relative neutron importance were all measured. The critical assembly, material reactivity worths, the surface material worth coefficient, and the delayed neutron fraction were all evaluated as benchmark experiment measurements. The reactor physics measurements are the focus of this paper; although for clarity the critical assembly benchmark specifications are briefly discussed.« less

Apparatus and process for the electrolytic reduction of uranium and plutonium oxides

DOEpatents

Poa, David S.; Burris, Leslie; Steunenberg, Robert K.; Tomczuk, Zygmunt

1991-01-01

An apparatus and process for reducing uranium and/or plutonium oxides to produce a solid, high-purity metal. The apparatus is an electrolyte cell consisting of a first container, and a smaller second container within the first container. An electrolyte fills both containers, the level of the electrolyte in the first container being above the top of the second container so that the electrolyte can be circulated between the containers. The anode is positioned in the first container while the cathode is located in the second container. Means are provided for passing an inert gas into the electrolyte near the lower end of the anode to sparge the electrolyte and to remove gases which form on the anode during the reduction operation. Means are also provided for mixing and stirring the electrolyte in the first container to solubilize the metal oxide in the electrolyte and to transport the electrolyte containing dissolved oxide into contact with the cathode in the second container. The cell is operated at a temperature below the melting temperature of the metal product so that the metal forms as a solid on the cathode.

Biosorption and biomineralization of uranium(VI) by Saccharomyces cerevisiae-Crystal formation of chernikovite.

PubMed

Zheng, Xin-Yan; Wang, Xiao-Yu; Shen, Yang-Hao; Lu, Xia; Wang, Tie-Shan

2017-05-01

Biosorption of heavy metal elements including radionuclides by microorganisms is a promising and effective method for the remediation of the contaminated places. The responses of live Saccharomyces cerevisiae in the toxic uranium solutions during the biosorption process and the mechanism of uranium biomineralization by cells were investigated in the present study. A novel experimental phenomenon that uranium concentrations have negative correlation with pH values and positive correlation with phosphate concentrations in the supernatant was observed, indicating that hydrogen ions, phosphate ions and uranyl ions were involved in the chernikovite precipitation actively. During the biosorption process, live cells desorb deposited uranium within the equilibrium state of biosorption system was reached and the phosphorus concentration increased gradually in the supernatant. These metabolic detoxification behaviours could significantly alleviate uranium toxicity and protect the survival of the cells better in the environment. The results of microscopic and spectroscopic analysis demonstrated that the precipitate on the cell surface was a type of uranium-phosphate compound in the form of a scale-like substance, and S. cerevisiae could transform the uranium precipitate into crystalline state-tetragonal chernikovite [H 2 (UO 2 ) 2 (PO 4 ) 2 ·8H 2 O]. Copyright © 2017 Elsevier Ltd. All rights reserved.

Uranium-mediated electrocatalytic dihydrogen production from water.

PubMed

Halter, Dominik P; Heinemann, Frank W; Bachmann, Julien; Meyer, Karsten

2016-02-18

Depleted uranium is a mildly radioactive waste product that is stockpiled worldwide. The chemical reactivity of uranium complexes is well documented, including the stoichiometric activation of small molecules of biological and industrial interest such as H2O, CO2, CO, or N2 (refs 1 - 11), but catalytic transformations with actinides remain underexplored in comparison to transition-metal catalysis. For reduction of water to H2, complexes of low-valent uranium show the highest potential, but are known to react violently and uncontrollably forming stable bridging oxo or uranyl species. As a result, only a few oxidations of uranium with water have been reported so far; all stoichiometric. Catalytic H2 production, however, requires the reductive recovery of the catalyst via a challenging cleavage of the uranium-bound oxygen-containing ligand. Here we report the electrocatalytic water reduction observed with a trisaryloxide U(III) complex [(((Ad,Me)ArO)3mes)U] (refs 18 and 19)--the first homogeneous uranium catalyst for H2 production from H2O. The catalytic cycle involves rare terminal U(IV)-OH and U(V)=O complexes, which have been isolated, characterized, and proven to be integral parts of the catalytic mechanism. The recognition of uranium compounds as potentially useful catalysts suggests new applications for such light actinides. The development of uranium-based catalysts provides new perspectives on nuclear waste management strategies, by suggesting that mildly radioactive depleted uranium--an abundant waste product of the nuclear power industry--could be a valuable resource.

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.

The apparent absence of chemical sensitivity in the 4d and 5d X-ray absorption spectroscopy of uranium compounds

DOE PAGES

Tobin, J. G.

2013-05-03

X-ray absorption spectroscopy (XAS) and related derivative measurements have been used to demonstrate that the Pu 5f states are strongly relativistic and have a 5f occupation number near 5. Owing to the success in this regime, it has been argued that the XAS measurements should be a powerful tool to probe 5f occupation variation, both as a function of elemental nature (actinide atomic number) and as a function of physical and chemical perturbation, e.g., oxidation state. We show that XAS and its related measurements fail in this latter aspect for a wide variety of uranium compounds and materials. Possible causesmore » will be discussed.« less

Distribution of uranium and some selected trace metals in human scalp hair from Balkans.

PubMed

Zunic, Z S; Tokonami, S; Mishra, S; Arae, H; Kritsananuwat, R; Sahoo, S K

2012-11-01

The possible consequences of the use of depleted uranium (DU) used in Balkan conflicts in 1995 and 1999 for the people and the environment of this reason need attention. The heavy metal content in human hair may serve as a good indicator of dietary, environmental and occupational exposures to the metal compounds. The present work summarises the distribution of uranium and some selected trace metals such as Mn, Ni, Cu, Zn, Sr, Cd and Cs in the scalp hair of inhabitants from Balkans exposed to DU directly and indirectly, i.e. Han Pijesak, Bratoselce and Gornja Stubla areas. Except U and Cs, all other metals were compared with the worldwide reported values of occupationally unexposed persons. Uranium concentrations show a wide variation ranging from 0.9 ± 0.05 to 449 ± 12 µg kg(-1). Although hair samples were collected from Balkan conflict zones, uranium isotopic measurement ((235)U/(238)U) shows a natural origin rather than DU.

Screening level model for ecological risk assessment at EF-Site Los Alamos National Laboratory, New Mexico. Final report

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

Alldredge, A.W.; Kirchner, T.B.; McLendon, T.

1995-12-01

In response to a paucity of data on the chemical toxicity of uranium to plants, a factorial experiment employing five uranium concentrations (0, 50, 500, 5000, 25000 ppm) and three moisture regimes (low, medium, high) was performed using three native grasses. Buchloe dactyloides (buffalograss-mid/late seral), Schizachyrium scoparium (little bluestem-late seral), and Aristida longiseta (purple threeawn-early/mid seral) were grown in monocultures and every mixture of two species under all combinations of uranium and moisture levels. This design allows for the analysis of uranium effects, as well as possible compound effects due to moisture stress. Several measures of plant health and viabilitymore » were made, including: percent emergence, survivability of seedlings and mature plants, root and shoot biomass, and the number and mass of inflorescences. No significant differences between uranium levels were observed in terms of emergence and seedling survival. Effects are evident for plant biomass, fecundity, and long-term survivability.« less

Quality control analytical methods: refractive index.

PubMed

Allen, Loyd V

2015-01-01

There are numerous analytical methods that can be utilized in a compounding pharmacy for a quality-assurance program. Since the index of refraction of a liquid/solution is a physical constant, it can be used to assist in identification of a substance, establish its purity, and, in some instances, to determine the concentration of an analyte in solution. This article serves as an introduction to refractive index and some applications of its use in a compounding program.

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.

A review of the high temperature oxidation of uranium oxides in molten salts and in the solid state to form alkali metal uranates, and their composition and properties

NASA Astrophysics Data System (ADS)

Griffiths, Trevor R.; Volkovich, Vladimir A.

An extensive review of the literature on the high temperature reactions (both in melts and in the solid state) of uranium oxides (UO 2, U 3O 8 and UO 3) resulting in the formation of insoluble alkali metal (Li to Cs) uranates is presented. Their uranate(VI) and uranate(V) compounds are examined, together with mixed and oxygen-deficient uranates. The reactions of uranium oxides with carbonates, oxides, per- and superoxides, chlorides, sulfates, nitrates and nitrites under both oxidising and non-oxidising conditions are critically examined and systematised, and the established compositions of a range of uranate(VI) and (V) compounds formed are discussed. Alkali metal uranates(VI) are examined in detail and their structural, physical, thermodynamic and spectroscopic properties considered. Chemical properties of alkali metal uranates(VI), including various methods for their reduction, are also reported. Errors in the current theoretical treatment of uranate(VI) spectra are identified and the need to develop routes for the preparation of single crystals is stressed.

Isolation and purification of macrocyclic components from Penicillium fermentation broth by high-speed counter-current chromatography.

PubMed

Gao, Xiang; Zhuang, Rongqiang; Guo, Jiannan; Bao, Jian; Fang, Meijuan; Liu, Yan; Xu, Pengxiang; Zhao, Yufen

2010-02-01

In this paper, high-speed counter-current chromatography (HSCCC), assisted with ESI-MS, was first successfully applied to the preparative separation of three macrolide antibiotics, brefeldin A (12.6 mg, 99.0%), 7'-O-formylbrefeldin A (6.5 mg, 95.0%) and 7'-O-acetylbrefeldin A (5.0 mg, 92.3%) from the crude extract of the microbe Penicillium SHZK-15. Considering the chemical nature and partition coefficient (K) values of the three target compounds, a two-step HSCCC isolation protocol was developed in order to obtain products with high purity. In the two-step method, the crude ethyl acetate extract was first fractionated and resulted in two peak fractions by HSCCC using solvent system n-hexane/ethyl acetate/methanol/water (HEMWat) (3:7:5:5 v/v/v/v), then purified using solvent systems HEMWat (3:5:3:5 v/v/v/v) and HEMWat (7:3:5:5 v/v/v/v) for each fraction. The purities and structures of the isolated compounds were determined by HPLC, X-ray crystallography, ESI-MS and NMR. The results demonstrated that HSCCC is a fast and efficient technique for systematic isolation of bioactive compounds from the microbes.

The Debye light scattering equation's scaling relation reveals the purity of synthetic dendrimers

NASA Astrophysics Data System (ADS)

Tseng, Hui-Yu; Chen, Hsiao-Ping; Tang, Yi-Hsuan; Chen, Hui-Ting; Kao, Chai-Lin; Wang, Shau-Chun

2016-03-01

Spherical dendrimer structures cannot be structurally modeled using conventional polymer models of random coil or rod-like configurations during the calibration of the static light scattering (LS) detectors used to determine the molecular weight (M.W.) of a dendrimer or directly assess the purity of a synthetic compound. In this paper, we used the Debye equation-based scaling relation, which predicts that the static LS intensity per unit concentration is linearly proportional to the M.W. of a synthetic dendrimer in a dilute solution, as a tool to examine the purity of high-generational compounds and to monitor the progress of dendrimer preparations. Without using expensive equipment, such as nuclear magnetic resonance or mass spectrometry, this method only required an affordable flow injection set-up with an LS detector. Solutions of the purified dendrimers, including the poly(amidoamine) (PAMAM) dendrimer and its fourth to seventh generation pyridine derivatives with size range of 5-9 nm, were used to establish the scaling relation with high linearity. The use of artificially impure mixtures of six or seven generations revealed significant deviations from linearity. The raw synthesized products of the pyridine-modified PAMAM dendrimer, which included incompletely reacted dendrimers, were also examined to gauge the reaction progress. As a reaction toward a particular generational derivative of the PAMAM dendrimers proceeded over time, deviations from the linear scaling relation decreased. The difference between the polydispersity index of the incompletely converted products and that of the pure compounds was only about 0.01. The use of the Debye equation-based scaling relation, therefore, is much more useful than the polydispersity index for monitoring conversion processes toward an indicated functionality number in a given preparation.

Release of 226Ra from uranium mill tailings by microbial Fe(III) reduction

USGS Publications Warehouse

Landa, E.R.; Phillips, E.J.P.; Lovley, D.R.

1991-01-01

Uranium mill tailings were anaerobically incubated in the presence of H2 with Alteromonas putrefaciens, a bacterium known to couple the oxidation of H2 and organic compounds to the reduction of Fe(III) oxides. There was a direct correlation between the extent of Fe(III) reduction and the accumulation of dissolved 226Ra. In sterile tailings in which Fe(III) was not reduced, there was negligible leaching of 226Ra. The behavior of Ba was similar to that of Ra in inoculated and sterile systems. These results demonstrate that under anaerobic conditions, microbial reduction of Fe(III) may result in the release of dissolved 226Ra from uranium mill tailings. ?? 1991.

Mathematical simulation of the amplification of 1790-nm laser radiation in a nuclear-excited He - Ar plasma containing nanoclusters of uranium compounds

NASA Astrophysics Data System (ADS)

Kosarev, V. A.; Kuznetsova, E. E.

2014-02-01

The possibility of applying dusty active media in nuclearpumped lasers has been considered. The amplification of 1790-nm radiation in a nuclear-excited dusty He - Ar plasma is studied by mathematical simulation. The influence of nanoclusters on the component composition of the medium and the kinetics of the processes occurring in it is analysed using a specially developed kinetic model, including 72 components and more than 400 reactions. An analysis of the results indicates that amplification can in principle be implemented in an active laser He - Ar medium containing 10-nm nanoclusters of metallic uranium and uranium dioxide.

Uranium Biomineralization By Natural Microbial Phosphatase Activities in the Subsurface

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

Taillefert, Martial

This project investigated the geochemical and microbial processes associated with the biomineralization of radionuclides in subsurface soils. During this study, it was determined that microbial communities from the Oak Ridge Field Research subsurface are able to express phosphatase activities that hydrolyze exogenous organophosphate compounds and result in the non-reductive bioimmobilization of U(VI) phosphate minerals in both aerobic and anaerobic conditions. The changes of the microbial community structure associated with the biomineralization of U(VI) was determined to identify the main organisms involved in the biomineralization process, and the complete genome of two isolates was sequenced. In addition, it was determined thatmore » both phytate, the main source of natural organophosphate compounds in natural environments, and polyphosphate accumulated in cells could also be hydrolyzed by native microbial population to liberate enough orthophosphate and precipitate uranium phosphate minerals. Finally, the minerals produced during this process are stable in low pH conditions or environments where the production of dissolved inorganic carbon is moderate. These findings suggest that the biomineralization of U(VI) phosphate minerals is an attractive bioremediation strategy to uranium bioreduction in low pH uranium-contaminated environments. These efforts support the goals of the SBR long-term performance measure by providing key information on "biological processes influencing the form and mobility of DOE contaminants in the subsurface".« less

Functionalization of carbon dioxide and carbon disulfide using a stable uranium(III) alkyl complex.

PubMed

Matson, Ellen M; Forrest, William P; Fanwick, Phillip E; Bart, Suzanne C

2011-04-06

A rare uranium(III) alkyl complex, Tp*(2)U(CH(2)Ph) (2) (Tp* = hydrotris(3,5-dimethylpyrazolyl)borate), was synthesized by salt metathesis from Tp*(2)UI (1) and KCH(2)Ph and fully characterized using (1)H NMR, infrared, and electronic absorption spectroscopies as well as X-ray crystallography. This complex has a uranium-carbon distance of 2.57(2) Å, which is comparable to other uranium alkyls reported. Treating this compound with either carbon dioxide or carbon disulfide results in insertion into the uranium-carbon bond to generate Tp*(2)U(κ(2)-O(2)CCH(2)Ph) (3) and Tp*(2)U(SC(S)CH(2)Ph) (4), respectively. These species, characterized spectroscopically and by X-ray crystallography, feature new carboxylate and dithiocarboxylate ligands. Analysis by electronic absorption spectroscopy supports the trivalent oxidation state of the uranium center in both of these derivatives. Addition of trimethylsilylhalides (Me(3)SiX; X = Cl, I) to 3 results in the release of the free silyl ester, Me(3)SiOC(O)CH(2)Ph, forming the initial uranium monohalide species, Tp*(2)UX, which can then be used over multiple cycles for the functionalization of carbon dioxide. © 2011 American Chemical Society

Molecular Mobility of an Amorphous Chiral Pharmaceutical Compound: Impact of Chirality and Chemical Purity.

PubMed

Viel, Quentin; Delbreilh, Laurent; Coquerel, Gérard; Petit, Samuel; Dargent, Eric

2017-08-17

A dielectric relaxation spectroscopy (DRS) study was performed to investigate the molecular mobility of amorphous chiral diprophylline (DPL). For this purpose, both racemic DPL and a single enantiomer of DPL were considered. After fast cooling from the melt at very low temperature (-140 °C), progressive heating below and above the glass transition (T g ≈ 37 °C) induces two secondary relaxations (γ- and δ-) and primary relaxations (α-) for both enantiomeric compositions. After chemical purification of our samples by means of cooling recrystallization, no γ-process could be detected by DRS. Hence, it was highlighted that the molecular mobility in the glassy state is influenced by the presence of theophylline (TPH), the main impurity in DPL samples. We also proved that the dynamic behavior of a single enantiomer and the racemic mixture of the same purified compound are quasi-identical. This study demonstrates that the relative stability and the molecular mobility of chiral amorphous drugs are strongly sensitive to chemical purity.

Exposure pathways and health effects associated with chemical and radiological toxicity of natural uranium: a review.

PubMed

Brugge, Doug; de Lemos, Jamie L; Oldmixon, Beth

2005-01-01

Natural uranium exposure derives from the mining, milling, and processing of uranium ore, as well as from ingestion of groundwater that is naturally contaminated with uranium. Ingestion and inhalation are the primary routes of entry into the body. Absorption of uranium from the lungs or digestive track is typically low but can vary depending on compound specific solubility. From the blood, two-thirds of the uranium is excreted in urine over the first 24 hours and up to 80% to 90% of uranium deposited in the bone leaves the body within 1.5 years. The primary health outcomes of concern documented with respect to uranium are renal, developmental, reproductive, diminished bone growth, and DNA damage. The reported health effects derive from experimental animal studies and human epidemiology. The Lowest Observed Adverse Effect Level (LOAEL) derived from animal studies is 50 microg/m3 for inhalation and 60 ug/kg body weight/day for ingestion. The current respiratory standard of the Occupational Safety and Health Administration (OSHA), 50 microg/m3, affords no margin of safety. Considering the safety factors for species and individual variation, the ingestion LOAEL corresponds to the daily consumption set by the World Health Organization Drinking Water Standard at 2 microg/L. Based on economic considerations, the United States Environmental Protection Agency maximum contaminant level is 30 microg/L. Further research is needed, with particular attention on the impact of uranium on indigenous populations, on routes of exposure in communities near uranium sites, on the combined exposures present at many uranium sites, on human developmental defects, and on health effects at or below established exposure standards.

Isolation of four phenolic compounds from Mangifera indica L. flowers by using normal phase combined with elution extrusion two-step high speed countercurrent chromatography.

PubMed

Shaheen, Nusrat; Lu, Yanzhen; Geng, Ping; Shao, Qian; Wei, Yun

2017-03-01

Two-step high speed countercurrent chromatography method, following normal phase and elution-extrusion mode of operation by using selected solvent systems, was introduced for phenolic compounds separation. Phenolic compounds including gallic acid, ethyl gallate, ethyl digallate and ellagic acid were separated from the ethanol extract of mango (Mangifera indica L.) flowers for the first time. In the first step, gallic acid of 3.7mg and ethyl gallate of 3.9mg with the purities of 98.87% and 99.55%, respectively, were isolated by using hexane-ethylacetate-methanol-water (4:6:4:6, v/v) in normal phase high speed countercurrent chromatography from 200mg of crude extract, while ethyl digallate and ellagic acid were collected in the form of mixture fraction. In the second step, further purification of the mixture was carried out with the help of another selected solvent system of dichloromethane-methanol-water (4:3:2, v/v) following elusion-extrusion mode of operation. Ethyl digallate of 3.8mg and ellagic acid of 5.7mg were separated well with high purities of 98.68% and 99.71%, respectively. The separated phenolic compounds were identified and confirmed by HPLC, UPLC-QTOF/ESI-MS, 1 H and 13 C NMR spectrometric analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Multiplet Splitting Effects on Core-Level Photoemission and Inverse-Photoemission Spectra of Uranium Intermetallic Compounds

NASA Astrophysics Data System (ADS)

Okada, Kozo

1999-03-01

The present paper discusses the role of U 5f-5f exchange interaction (J) in the inverse photoemission spectrum (IPES) and the U 4f x-ray photoemission spectrum (XPS) of uranium intermetallic compounds. The origin of the broad main peak in the IPES of UPd3 and UPd2Al3, for instance, is ascribed to the exchange coupling effects of 5f electrons. In other words, whether the ground state is of high-spin or of low-spin is directly reflected in the width of the IPES. On the other hand, the interpretation for the U 4f photoemission spectrum is not so greatly influenced by J. The full-multiplet calculations are also performed for an U4+ ion for comparison.

Dissolution of synthetic uranium dibutyl phosphate deposits in oxidizing and reducing chemical formulations.

PubMed

Rufus, A L; Sathyaseelan, V S; Narasimhan, S V; Velmurugan, S

2013-06-15

Permanganate and nitrilotriacetic acid (NTA) based dilute chemical formulations were evaluated for the dissolution of uranium dibutyl phosphate (U-DBP), a compound that deposits over the surfaces of nuclear reprocessing plants and waste storage tanks. A combination of an acidic, oxidizing treatment (nitric acid with permanganate) followed by reducing treatment (NTA based formulation) efficiently dissolved the U-DBP deposits. The dissolution isotherm of U-DBP in its as precipitated form followed a logarithmic fit. The same chemical treatment was also effective in dissolving U-DBP coated on the surface of 304-stainless steel, while resulting in minimal corrosion of the stainless steel substrate material. Investigation of uranium recovery from the resulting decontamination solutions by ion exchange with a bed of mixed anion and cation resins showed quantitative removal of uranium. Copyright © 2013 Elsevier B.V. All rights reserved.

Study of behaviors of aluminum overlayers deposited on uranium via AES, EELS, and XPS

NASA Astrophysics Data System (ADS)

Liu, Kezhao; Luo, Lizhu; Zhou, Wei; Yang, Jiangrong; Xiao, Hong; Hong, Zhanglian; Yang, Hui

2013-04-01

Aluminum overlayers on uranium were prepared by sputtering at room temperature in an ultra-high vacuum chamber. The growth mode of aluminum overlayers and behaviors of the Al/U interface reaction were studied in situ by auger electron spectroscopy, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy. The results suggested that the interdiffusion took place at the Al/U interface during the initial stage of deposition. The U4f spectra of the Al/U interface showed strong correlation satellites at binding energies of 380.4 and 392.7 eV and plasma loss features at 404.2 eV, respectively. The interactions between aluminum and uranium yielded the intermetallic compound of UAlx, inducing the shift to a low binding energy for Al2p peaks. The results indicated that aluminum overlayers were formed on the uranium by sputtering in an island growth mode.

An off-line method to characterize the fission product release from uranium carbide-target prototypes developed for SPIRAL2 project

NASA Astrophysics Data System (ADS)

Hy, B.; Barré-Boscher, N.; Özgümüs, A.; Roussière, B.; Tusseau-Nenez, S.; Lau, C.; Cheikh Mhamed, M.; Raynaud, M.; Said, A.; Kolos, K.; Cottereau, E.; Essabaa, S.; Tougait, O.; Pasturel, M.

2012-10-01

In the context of radioactive ion beams, fission targets, often based on uranium compounds, have been used for more than 50 years at isotope separator on line facilities. The development of several projects of second generation facilities aiming at intensities two or three orders of magnitude higher than today puts an emphasis on the properties of the uranium fission targets. A study, driven by Institut de Physique Nucléaire d'Orsay (IPNO), has been started within the SPIRAL2 project to try and fully understand the behavior of these targets. In this paper, we have focused on five uranium carbide based targets. We present an off-line method to characterize their fission product release and the results are examined in conjunction with physical characteristics of each material such as the microstructure, the porosity and the chemical composition.

Calixarene cleansing formulation for uranium skin contamination.

PubMed

Phan, Guillaume; Semili, Naïma; Bouvier-Capely, Céline; Landon, Géraldine; Mekhloufi, Ghozlene; Huang, Nicolas; Rebière, François; Agarande, Michelle; Fattal, Elias

2013-10-01

An oil-in-water cleansing emulsion containing calixarene molecule, an actinide specific chelating agent, was formulated in order to improve the decontamination of uranium from the skin. Commonly commercialized cosmetic ingredients such as surfactants, mineral oil, or viscosifying agents were used in preparing the calixarene emulsion. The formulation was characterized in terms of size and apparent viscosity measurements and then was tested for its ability to limit uranyl ion permeation through excoriated pig-ear skin explants in 24-h penetration studies. Calixarene emulsion effectiveness was compared with two other reference treatments consisting of DTPA and EHBP solutions. Application of calixarene emulsion induced the highest decontamination effect with an 87% decrease in uranium diffusion flux. By contrast, EHBP and DTPA solutions only allowed a 50% and 55% reduction of uranium permeation, respectively, and had the same effect as a simple dilution of the contamination by pure water. Uranium diffusion decrease was attributed to uranyl ion-specific chelation by calixarene within the formulation, since no significant effect was obtained after application of the same emulsion without calixarene. Thus, calixarene cleansing emulsion could be considered as a promising treatment in case of accidental contamination of the skin by highly diffusible uranium compounds.

In situ ligand synthesis with the UO{sub 2}{sup 2+} cation under hydrothermal conditions

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

Frisch, Mark; Cahill, Christopher L.; Geophysical Laboratory, Carnegie Institution of Washington, Washington, DC

A novel uranium (VI) coordination polymer, (UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(C{sub 5}H{sub 6}NO{sub 3}){sub 2} (1), has been prepared under the hydrothermal reaction of uranium nitrate hexahydrate and L-pyroglutamic acid. Compound 1 (monoclinic, C2/c, a=22.541(6) A, b=5.7428(15) A, c=15.815(4) A, {beta}=119.112(4){sup o}, Z=4, R{sub 1}=0.0237, wR{sub 2}=0.0367) consists of uranium pentagonal bipyramids linked via L-pyroglutamate and oxalate anions to form an overall two-dimensional (2D) structure. With the absence of oxalic acid within the starting materials, the oxalate anions are hypothesized to form in situ whereby decarboxylation of L-pyroglutamic acid occurs followed by coupling of CO{sub 2} to form the oxalatemore » linkages as observed in the crystal structure. Addition of copper (II) to this system appears to promote oxalate formation in that synthetic moolooite (Cu(C{sub 2}O{sub 4}).nH{sub 2}O; 0{<=}n{<=}1) and a known uranyl oxalate [(UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(OH){sub 2}(H{sub 2}O){sub 2}.H{sub 2}O], co-crystallize in significant quantity. Compound 1 exhibits the characteristic uranyl emission spectrum upon either direct uranyl excitation or ligand excitation, the latter of which shows an increase in relative intensity. This subsequent increase in the intensity indicates an energy transfer from the ligand to the uranyl cations thus illustrating an example of the antenna effect in the solid state. - Graphical abstract: A novel homometallic coordination polymer (UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(C{sub 5}H{sub 6}NO{sub 3}){sub 2}, in the uranium-L-pyroglutamic acid system has been synthesized under hydrothermal conditions. The title compound consists of uranium pentagonal bipyramids bridged through both L-pyroglutamate and oxalate linkages to produce a 3D crystal structure. The oxalate anions are theorized to result from decarboxylation of L-pyroglutamic acid followed by subsequent coupling of CO{sub 2}.« less

Nitrogen reduction and functionalization by a multimetallic uranium nitride complex

NASA Astrophysics Data System (ADS)

Falcone, Marta; Chatelain, Lucile; Scopelliti, Rosario; Živković, Ivica; Mazzanti, Marinella

2017-07-01

Molecular nitrogen (N2) is cheap and widely available, but its unreactive nature is a challenge when attempting to functionalize it under mild conditions with other widely available substrates (such as carbon monoxide, CO) to produce value-added compounds. Biological N2 fixation can do this, but the industrial Haber-Bosch process for ammonia production operates under harsh conditions (450 degrees Celsius and 300 bar), even though both processes are thought to involve multimetallic catalytic sites. And although molecular complexes capable of binding and even reducing N2 under mild conditions are known, with co-operativity between metal centres considered crucial for the N2 reduction step, the multimetallic species involved are usually not well defined, and further transformation of N2-binding complexes to achieve N-H or N-C bond formation is rare. Haber noted, before an iron-based catalyst was adopted for the industrial Haber-Bosch process, that uranium and uranium nitride materials are very effective heterogeneous catalysts for ammonia production from N2. However, few examples of uranium complexes binding N2 are known, and soluble uranium complexes capable of transforming N2 into ammonia or organonitrogen compounds have not yet been identified. Here we report the four-electron reduction of N2 under ambient conditions by a fully characterized complex with two UIII ions and three K+ centres held together by a nitride group and a flexible metalloligand framework. The addition of H2 and/or protons, or CO to the resulting complex results in the complete cleavage of N2 with concomitant N2 functionalization through N-H or N-C bond-forming reactions. These observations establish that a molecular uranium complex can promote the stoichiometric transformation of N2 into NH3 or cyanate, and that a flexible, electron-rich, multimetallic, nitride-bridged core unit is a promising starting point for the design of molecular complexes capable of cleaving and functionalizing N2 under mild conditions.

Spectroscopic studies of uranium species for environmental decontamination applications

NASA Astrophysics Data System (ADS)

Eng, Charlotte

After the Cold War, Department of Energy began to concentrate its efforts on cleanup of former nuclear material processing facilities, especially uranium-contaminated groundwater and soil. This research aims to study uranium association to both organic and inorganic compounds found in the contaminated environment in the hopes that the information gathered can be applied to the development and optimization of cost-effective remediation techniques. Spectroscopic and electrochemical methods will be employed to examine the behavior of uranium in given conditions to further our understanding of its impact on the environment. Uranium found in groundwater and soil bind with various ligands, especially organic ligands present in the environment due to natural sources (e.g. metabolic by-products or degradation of plants and animals) or man-made sources (e.g. chelating agents used in operating or cleanup of uranium processing facilities). We selected reasonable analogs of naturally occurring matter and studied their structure, chemical and electrochemical behavior and found that the structure of uranyl complexes depends heavily on the nature of the ligand and environmental factors such as pH. Association of uranium-organic complexes with anaerobic bacteria, Clostridium sp. was studied to establish if the bacteria can effectively bioreduce uranium while going through normal bacterial activity. It was found that the nature of the organic ligand affected the bioavailability and toxicity of the uranium on the bacteria. In addition, we have found that the type of iron corrosion products and uranyl species present on the surface of corroded steel depended on various environmental factors, which subsequently affected the removal rate of uranium by a citric acid/hydrogen peroxide/deionized water cleaning process. The method was found to remove uranium from only the topmost corrosion layers and residual uranium could be found (a) deeper in the corrosion layers where it is occluded by the steel corrosion products or (b) in areas where the dissolved uranium/iron species, the products generated by the dissolution power of citric acid, was not properly rinsed away.

Reconnaissance of uranium and copper deposits in parts of New Mexico, Colorado, Utah, Idaho, and Wyoming

USGS Publications Warehouse

Gott, Garland B.; Erickson, Ralph L.

1952-01-01

Because of the common association of uranium and copper in several of the commercial uranium deposits in the Colorado Plateau Province, a reconnaissance was made of several known deposits of copper disseminated through sandstone to determine whether they might be a source of uranium. In order to obtain more information regarding the relationship between copper, uranium and carbonaceous materials, some of the uraniferious asphaltrite deposits in the Shinarump conglomerate along the west flank of the San Rafael Swell were also investigated briefly. During this reconnaissance 18 deposits were examined in New Mexico, eight in Utah, two in Idaho, and one each in Wyoming and Colorado. No uranium deposits of commercial grade are associated with the copper deposits that were examined. The uraniferous asphaltites in the Shinarump conglomerate of Triassic age on the west flank of the San Rafael Swell, however, are promising from the standpoint of commercial uranium production. Spectrographic analyses of crude oil, asphalt, and bituminous shales show a rather consistent suite of trace metals including vanadium, nickel, copper, cobalt, chromium, lead zinc, and molybdenum. The similarity of the metal assemblage, including uranium of the San Rafael Swell asphaltites, to the metal assemblage in crude oil and other bituminous materials suggests that these metals were concentrated in the asphaltites from petroleum. However, the hypothesis that uranium minerals were already present before the hydrocarbons were introduced and that some sort of replacement or uranium minerals by carbon compounds was effected after the petroleum migrated into the uranium deposit should not be disregarded. The widespread association of uranium with asphaltic material suggests that it also may have been concentrated by some agency connected with the formation of petroleum. The problem of the association of uranium and other trace metals with hydrocarbons should be studied further both in the field and in the laboratory.

Actinide Foil Production for MPACT Research

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

Beller, Denis

Sensitive fast-neutron detectors are required for use in lead slowing down spectrometry (LSDS), an active interrogation technique for used nuclear fuel assay for Materials Protection, Accounting, and Controls Technologies (MPACT). During the past several years UNLV sponsored a research project at RPI to investigate LSDS; began development of fission chamber detectors for use in LSDS experiments in collaboration with INL, LANL, and Oregon State U.; and participated in a LSDS experiment at LANL. In the LSDS technique, research has demonstrated that these fission chamber detectors must be sensitive to fission energy neutrons but insensitive to thermal-energy neutrons. Because most systemsmore » are highly sensitive to large thermal neutron populations due to the well-known large thermal cross section of 235U, even a miniscule amount of this isotope in a fission chamber will overwhelm the small population of higher-energy neutrons. Thus, fast-fission chamber detectors must be fabricated with highly depleted uranium (DU) or ultra-pure thorium (Th), which is about half as efficient as DU. Previous research conducted at RPI demonstrated that the required purity of DU for assay of used nuclear fuel using LSDS is less than 4 ppm 235U, material that until recently was not available in the U.S. In 2009 the PI purchased 3 grams of ultra-depleted uranium (uDU, 99.99998% 238U with just 0.2 ± 0.1 ppm 235U) from VNIIEF in Sarov, Russia. We received the material in the form of U3O8 powder in August of 2009, and verified its purity and depletion in a FY10 MPACT collaboration project. In addition, chemical processing for use in FC R&D was initiated, fission chamber detectors and a scanning alpha-particle spectrometer were developed, and foils were used in a preliminary LSDS experiment at a LANL/LANSCE in Sept. of 2010. The as-received U3O8 powder must be chemically processed to convert it to another chemical form while maintaining its purity, which then must be used to electro-deposit U or UO2 in extremely thin layers (1 to 2 mg/cm2) on various media such as films, foils, or discs. After many months of investigation and trials in FY10 and 11, UNLV researchers developed a new method to produce pure UO2 deposits on foils using a unique approach, which has never been demonstrated, that involves dissolution of U3O8 directly into room temperature ionic liquid (RTIL) followed by electrodeposition from the RTIL-uDU solution (Th deposition from RTIL had been previously demonstrated). The high-purity dissolution of the U3O8 permits the use of RTIL solutions for deposition of U on metal foils in layers without introducing contamination. In FY10 and early FY11 a natural U surrogate for the uDU was used to investigate this and other techniques. In this research project UNLV will deposit directly from RTIL to produce uDU and Th foils devoid of possible contaminants. After these layers have been deposited, they will be examined for purity and uniformity. UNLV will complete the development and demonstration of the RTIL technology/ methodology to prepare uDU and Th samples for use in constructing fast-neutron detectors. Although this material was purchased for use in research using fast-fission chamber detectors for active inspection techniques for MPACT, it could also contribute to R&D for other applications, such as cross section measurements or neutron spectroscopy for national security« less

ISOTOPE FRACTIONATION PROCESS

DOEpatents

Clewett, G.H.; Lee, DeW.A.

1958-05-20

A new method is described for isotopic enrichment of uranium. It has been found that when an aqueous acidic solution of ionic tetravalent uraniunn is contacted with chelate complexed tetravalent uranium, the U/sup 238/ preferentially concentrates in the complexed phase while U/sup 235/ concentrates in the ionic phase. The effect is enhanced when the chelate compound is water insoluble and is dissolved in a water-immiscible organic solvent. Cupferron is one of a number of sultable complexing agents, and chloroform is a suitable organic solvent.

238U Mössbauer study on the magnetic properties of uranium-based heavy fermion superconductors

NASA Astrophysics Data System (ADS)

Tsutsui, Satoshi; Nakada, Masami; Nasu, Saburo; Haga, Yoshinori; Honma, Tetsuo; Yamamoto, Etsuji; Ohkuni, Hitoshi; Ōnuki, Yoshichika

2000-07-01

We have performed 238U Mössbauer spectroscopy of uranium-based heavy fermion superconductors, UPd2Al3 and URu2Si2, in order to investigate their physical properties, mainly their magnetic properties. The slow relaxation of magnetic hyperfine interaction in a paramagnetic state and the static hyperfine field has been observed in an antiferromagnetic ordered state for each compound. The line-widths have maximum at their characteristic temperatures where their magnetic susceptibilities have maximum values.

Constitutional studies on carbide nuclear fuels for fast breeder reactors. III. The uranium-barium-carbon ternary system at 1400°C, with observations on the uranium-strontium-carbon system

NASA Astrophysics Data System (ADS)

Peatfield, M.; Brett, N. H.; Potter, P. E.

1980-03-01

The ternary system U-Ba-C has been examined at 1400°C and the solid-state compatibility lines established. No compound formation was found to occur and solubility effects were found to be minimal. A tentative examination of compositions in the U-Sr-C system indicates that it is of a similar form to that of the U-Ba-C system.

SEPARATION OF URANIUM HEXAFLUORIDE FROM ORGANIC FLUORO COMPOUNDS

DOEpatents

Libby, W.F.

1958-10-01

A method is presented for removing perfiuoroorganic compounds such as C/ sub 7/F/sub 16/ from UF/sub 6/. The physical and chemical properties of the perfluoro compounds are such as to render their removal from UF/sub 6/ difficulty by conventional techniques. The mixture containing UF/sub 6/ and the perfluoro compounds is pyrolyzed in an inert container at high temperature and pressure. The properties of the products obtained by pyrolysis differ from the properties of UF/sub 6/ to a sufficient degree to render their separation possible by ordinary methods.

SEPARATION PROCESS FOR PROTACTINIUM AND COMPOUNDS THEREOF

DOEpatents

Van Winkle, A.

1959-07-21

The separation of protactinium from aqueous solutions from its mixtures with thorium, uranium and fission products is described. The process for the separation comprises preparing an ion nitric acid solution containing protactinium in the pentavalent state and contacting the solution with a fluorinated beta diketone, such as trifluoroacetylacetone, either alone or as an organic solvent solution to form a pentavalent protactinium chelate compound. When the organic solvent is present the chelate compound is extracted; otherwise it is separated by filtration.

SOME GEOCHEMICAL METHODS OF URANIUM EXPLORATION

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

Illsley, C.T.; Bills, C.W.; Pollock, J.W.

Geochemical research and development projects were carried on to provide basic information which may be applied to exploration or general studies of uranium geology. The applications and limitations of various aspects of geochemistry to uranium geological problems are considerd. Modifications of existing analytical techniques were made and tested in the laboratory and in the field. These include rapid quantitative determination of unranium in water, soil and peat, and of trace amounts of sulfate and phosphate in water. Geochemical anomaly'' has been defined as a significant departure from the average abundance background of an element where the distribution has not beenmore » disturbed by mineralization. The detection and significance of geocthemical anomalies are directly related to the mobility of the element being sought in the zone of weathering. Mobility of uranium is governed by complex physical, chemical, and biological factors. For uranium anomalies in surface materils, the chemicaly factors affecting mobility are the most sigificant. The effects of pH, solubility, coprecipitution, adsorption complexion, or compound formation are discussed in relation to anomalies detected in water, soil, and stream sediments. (auth)« less

Uranium-mediated electrocatalytic dihydrogen production from water

NASA Astrophysics Data System (ADS)

Halter, Dominik P.; Heinemann, Frank W.; Bachmann, Julien; Meyer, Karsten

2016-02-01

Depleted uranium is a mildly radioactive waste product that is stockpiled worldwide. The chemical reactivity of uranium complexes is well documented, including the stoichiometric activation of small molecules of biological and industrial interest such as H2O, CO2, CO, or N2 (refs 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11), but catalytic transformations with actinides remain underexplored in comparison to transition-metal catalysis. For reduction of water to H2, complexes of low-valent uranium show the highest potential, but are known to react violently and uncontrollably forming stable bridging oxo or uranyl species. As a result, only a few oxidations of uranium with water have been reported so far; all stoichiometric. Catalytic H2 production, however, requires the reductive recovery of the catalyst via a challenging cleavage of the uranium-bound oxygen-containing ligand. Here we report the electrocatalytic water reduction observed with a trisaryloxide U(III) complex [((Ad,MeArO)3mes)U] (refs 18 and 19)—the first homogeneous uranium catalyst for H2 production from H2O. The catalytic cycle involves rare terminal U(IV)-OH and U(V)=O complexes, which have been isolated, characterized, and proven to be integral parts of the catalytic mechanism. The recognition of uranium compounds as potentially useful catalysts suggests new applications for such light actinides. The development of uranium-based catalysts provides new perspectives on nuclear waste management strategies, by suggesting that mildly radioactive depleted uranium—an abundant waste product of the nuclear power industry—could be a valuable resource.

Potassium N-Iodo p-Toluenesulfonamide (TsNIK, Iodamine-T): A New Reagent for the Oxidation of Hydrazones to Diazo Compounds

PubMed Central

Nicolle, Simon M; Moody, Christopher J

2014-01-01

A new reagent for the oxidation of hydrazones to diazo compounds is described. N-Iodo p-toluenesulfonamide (TsNIK, iodamine-T) allows the preparation of α-diazoesters, α-diazoamides, α-diazoketones and α-diazophosphonates in good yield and in high purity after a simple extractive work-up. α-Diazoesters were also obtained in high yield from the corresponding ketones through a one-pot process of hydrazone formation/oxidation. PMID:24615944

MOD silver metallization for photovoltaics

NASA Technical Reports Server (NTRS)

Vest, G. M.; Vest, R. W.

1985-01-01

The feasibility of utilizing metallo-organic decomposition (MOD) silver inks were investigated for front contact metallization of solar cells. Generic synthesis procedures were developed for all metallo-organic compounds investigated. Silver neodecanoate was found to be the most suitable silver metallo-organic compound for use in thick film inks, but the quality of the inks was found to be highly dependent on its purity. Although neither the process nor inks were completely optimized for solar cell front contact metallization, they show great promise for this application.

49 CFR 176.84 - Other requirements for stowage and segregation for cargo vessels and passenger vessels.

Code of Federal Regulations, 2012 CFR

2012-10-01

... liquids. 29 Stow “away from” ammonium compounds. 30 Stow “away from” animal or vegetable oils. 31 Stow...” alkaline compounds.2 54 Stow “separated from” animal or vegetable oils. 55 Stow “separated from” ammonia... applies. 130 Stowage Category A applies, except for uranyl nitrate hexahydrate solution, uranium metal...

49 CFR 176.84 - Other requirements for stowage and segregation for cargo vessels and passenger vessels.

Code of Federal Regulations, 2011 CFR

2011-10-01

... liquids. 29 Stow “away from” ammonium compounds. 30 Stow “away from” animal or vegetable oils. 31 Stow...” alkaline compounds.2 54 Stow “separated from” animal or vegetable oils. 55 Stow “separated from” ammonia... applies. 130 Stowage Category A applies, except for uranyl nitrate hexahydrate solution, uranium metal...

METHOD OF PRODUCING URANIUM

DOEpatents

Foster, L.S.; Magel, T.T.

1958-05-13

A modified process is described for the production of uranium metal by means of a bomb reduction of UF/sub 4/. Difficulty is sometimes experienced in obtaining complete separation of the uranium from the slag when the process is carried out on a snnall scale, i.e., for the production of 10 grams of U or less. Complete separation may be obtained by incorporating in the reaction mixture a quantity of MnCl/sub 2/, so that this compound is reduced along with the UF/sub 4/ . As a result a U--Mn alloy is formed which has a melting point lower than that of pure U, and consequently the metal remains molten for a longer period allowing more complete separation from the slag.

Laser removal of loose uranium compound contamination from metal surfaces

NASA Astrophysics Data System (ADS)

Roberts, D. E.; Modise, T. S.

2007-04-01

Pulsed laser removal of surface contamination of uranyl nitrate and uranium dioxide from stainless steel has been studied. Most of the loosely bound contamination has been removed at fluence levels below 0.5 J cm -2, leaving about 5% fixed contamination for uranyl nitrate and 15% for uranium dioxide. Both alpha and beta activities are then sufficiently low that contaminated objects can be taken out of a restricted radiation area for re-use. The ratio of beta to alpha activity is found to be a function of particle size and changes during laser removal. In a separate experiment using technetium-99m, the collection of removed radioactivity in the filter was studied and an inventory made of removed and collected contamination.

A study on artificial rare earth (RE2O3) based neutron absorber.

PubMed

Kim, Kyung-O; Kyung Kim, Jong

2015-11-01

A new concept of a neutron absorption material (i.e., an artificial rare earth compound) was introduced for criticality control in a spent fuel storage system. In particular, spent nuclear fuels were considered as a potential source of rare earth elements because the nuclear fission of uranium produces a full range of nuclides. It was also found that an artificial rare earth compound (RE2O3) as a High-Level Waste (HLW) was naturally extracted from pyroprocessing technology developed for recovering uranium and transuranic elements (TRU) from spent fuels. In this study, various characteristics (e.g., activity, neutron absorption cross-section) were analyzed for validating the application possibility of this waste compound as a neutron absorption material. As a result, the artificial rare earth compound had a higher neutron absorption probability in the entire energy range, and it can be used for maintaining sub-criticality for more than 40 years on the basis of the neutron absorption capability of Boral™. Therefore, this approach is expected to vastly improve the efficiency of radioactive waste management by simultaneously keeping HLW and spent nuclear fuel in a restricted space. Copyright © 2015 Elsevier Ltd. All rights reserved.

REDUCTION OF INORGANIC COMPOUNDS WITH MOLECULAR HYDROGEN BY MICROCOCCUS LACTILYTICUS I.

PubMed Central

Woolfolk, C. A.; Whiteley, H. R.

1962-01-01

Woolfolk, C. A. (University of Washington, Seattle) and H. R. Whiteley. Reduction of inorganic compounds with molecular hydrogen by Micrococcus lactilyticus. I. Stoichiometry with compounds of arsenic, selenium, tellurium, transition and other elements. J. Bacteriol. 84:647–658. 1962.—Extracts of Micrococcus lactilyticus (Veillonella alcalescens) oxidize molecular hydrogen at the expense of certain compounds of arsenic, bismuth, selenium, tellurium, lead, thallium, vanadium, manganese, iron, copper, molybdenum, tungsten, osmium, ruthenium, gold, silver, and uranium, as well as molecular oxygen. Chemical and manometric data indicate that the following reductions are essentially quantitative: arsenate to arsenite, pentavalent and trivalent bismuth to the free element, selenite via elemental selenium to selenide, tellurate and tellurite to tellurium, lead dioxide and manganese dioxide to the divalent state, ferric to ferrous iron, osmium tetroxide to osmate ion, osmium dioxide and trivalent osmium to the metal, uranyl uranium to the tetravalent state, vanadate to the level of vanadyl, and polymolybdate ions to molybdenum blues with an average valence for molybdenum of +5. The results of a study of certain other hydrogenase-containing bacteria with respect to their ability to carry out some of the same reactions are also presented. PMID:14001842

DUF6 Guide

Science.gov Websites

and the environment. The Guide provides basic information about the properties of uranium compounds understand the unique challenges involved in managing DOE's inventory of depleted UF6 in a safe and efficient

The study of natural and artificial radionuclides incorporation in teeth and head bones of animals lived nearby Caetité uranium mine, Brazil.

PubMed

Walencik-Łata, A; Kozłowska, B; Mietelski, J W; Szufa, K; Freire, F D; Souza, S O

2016-10-01

This study aimed at assessing the incorporation of radionuclides in animals in the proximity of the uranium mine in Caetité, Brazil. In 2014, samples of bovine and equine teeth and skull bones were collected and their contents of natural and artificial isotopes were assessed using nuclear spectrometry techniques. Gamma ray emission from 226,228 Ra and 40 K isotopes was determined using high-purity germanium (HPGe) spectrometry, 90 Sr radioactivity was measured with liquid scintillation, and 234,238 U, 232,230,228 Th, 210 Po and 239+240 Pu radioactivity was assessed with alpha-spectrometry. Prior to the measurements, sample dissolutions and isotope separations were performed. Our results indicate a high 228 Th isotope content in the skull bones and the teeth of animals, up to 179 Bq per kg of ash. The 226 Ra and 228 Ra concentrations were slightly lower. Activity concentrations of other isotopes were significantly lower or below the detection limit. We could not identify sources of technologically enhanced levels of 228 Ra in the area we investigated; therefore we suggest that their origin is natural. Copyright © 2016 Elsevier Ltd. All rights reserved.

PLUTONIUM PURIFICATION PROCESS EMPLOYING THORIUM PYROPHOSPHATE CARRIER

DOEpatents

King, E.L.

1959-04-28

The separation and purification of plutonium from the radioactive elements of lower atomic weight is described. The process of this invention comprises forming a 0.5 to 2 M aqueous acidffc solution containing plutonium fons in the tetravalent state and elements with which it is normally contaminated in neutron irradiated uranium, treating the solution with a double thorium compound and a soluble pyrophosphate compound (Na/sub 4/P/sub 2/O/sub 7/) whereby a carrier precipitate of thorium A method is presented of reducing neptunium and - trite is advantageous since it destroys any hydrazine f so that they can be removed from solutions in which they are contained is described. In the carrier precipitation process for the separation of plutonium from uranium and fission products including zirconium and columbium, the precipitated blsmuth phosphate carries some zirconium, columbium, and uranium impurities. According to the invention such impurities can be complexed and removed by dissolving the contaminated carrier precipitate in 10M nitric acid, followed by addition of fluosilicic acid to about 1M, diluting the solution to about 1M in nitric acid, and then adding phosphoric acid to re-precipitate bismuth phosphate carrying plutonium.

Metrological approaches to organic chemical purity: primary reference materials for vitamin D metabolites.

PubMed

Nelson, Michael A; Bedner, Mary; Lang, Brian E; Toman, Blaza; Lippa, Katrice A

2015-11-01

Given the critical role of pure, organic compound primary reference standards used to characterize and certify chemical Certified Reference Materials (CRMs), it is essential that associated mass purity assessments be fit-for-purpose, represented by an appropriate uncertainty interval, and metrologically sound. The mass fraction purities (% g/g) of 25-hydroxyvitamin D (25(OH)D) reference standards used to produce and certify values for clinical vitamin D metabolite CRMs were investigated by multiple orthogonal quantitative measurement techniques. Quantitative (1)H-nuclear magnetic resonance spectroscopy (qNMR) was performed to establish traceability of these materials to the International System of Units (SI) and to directly assess the principal analyte species. The 25(OH)D standards contained volatile and water impurities, as well as structurally-related impurities that are difficult to observe by chromatographic methods or to distinguish from the principal 25(OH)D species by one-dimensional NMR. These impurities have the potential to introduce significant biases to purity investigations in which a limited number of measurands are quantified. Combining complementary information from multiple analytical methods, using both direct and indirect measurement techniques, enabled mitigation of these biases. Purities of 25(OH)D reference standards and associated uncertainties were determined using frequentist and Bayesian statistical models to combine data acquired via qNMR, liquid chromatography with UV absorbance and atmospheric pressure-chemical ionization mass spectrometric detection (LC-UV, LC-ACPI-MS), thermogravimetric analysis (TGA), and Karl Fischer (KF) titration.

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

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.

Determination of trace level thorium and uranium in high purity gadolinium sulfate using ICP-MS with solid-phase chromatographic extraction resins

NASA Astrophysics Data System (ADS)

Ito, S.; Takaku, Y.; Ikeda, M.; Kishimoto, Y.

2018-01-01

The Super Kamiokand-Gadolinium (SK-Gd) project is the upgrade of the Super-Kamiokande (SK) detector in order to discover Supernova Relic Neutrinos (SRNs) by loading 0.2% of Gd2(SO4)3 into a 50 kton of the SK water tank. In order to continue solar neutrino measurement with low energy threshold at ˜3.5 MeV, main radioactive contamination, U and Th in Gd2(SO4)3, should be purified before loading. We developed solid-phase extraction technique to measure low concentration of U and Th in Gd2(SO4)3 by ICP-MS. The extraction technique and current status will be presented.

Redox bias in loss of ignition moisture measurement for relatively pure plutonium-bearing oxide materials.

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

Eller, P. G.; Stakebake, J. L.; Cooper, T. D.

2001-01-01

This paper evaluates potential analytical bias in application of the Loss on Ignition (LOI) technique for moisture measurement to relatively pure (plutonium assay of 80 wt.% or higher) oxides containing uranium that have been stabilized according to stabilization and storage standard DOE-STD-3013-2000 (STD-3013). An immediate application is to Rocky Flats (RF) materials derived from highgrade metal hydriding separations subsequently treated by multiple calcination cycles. Specifically evaluated are weight changes due to oxidatiodreduction of multivalent impurity oxides that could mask true moisture equivalent content measurement. Process knowledge and characterization of materials representing complex-wide materials to be stabilized and packaged according tomore » STD-3013, and particularly for the immediate RF target stream, indicate that oxides of uranium, iron and gallium are the only potential multivalent constituents expected to be present above 0.5 wt.%. The evaluation shows that of these constituents, with few exceptions, only uranium oxides can be present at a sufficient level to produce weight gain biases significant with respect to the LO1 stability test. In general, these formerly high-value, high-actinide content materials are reliably identifiable by process knowledge and measurement. Si&icant bias also requires that UO1 components remain largely unoxidized after calcination and are largely converted to U30s clsning LO1 testing at only slightly higher temperatures. Based on wellestablished literature, it is judged unlikely that this set of conditions will be realized in practice. We conclude that it is very likely that LO1 weight gain bias will be small for the immediate target RF oxide materials containing greater than 80 wt.% plutonium plus a much smaller uranium content. Recommended tests are in progress to confum these expectations and to provide a more authoritative basis for bounding LO1 oxidatiodreduction biases. LO1 bias evaluation is more difficult for lower purity materials and for fuel-type uranium-plutonium oxides. However, even in these cases testing may show that bias effects are manageable.« less

Design and Growth of Novel Compounds for Radiation Sensors: Multinary Chalcogenides

NASA Technical Reports Server (NTRS)

Singh, N. B.; Su, Ching-Hua; Nagaradona, Teja; Arnold, Brad; Choa, Fow-Sen

2016-01-01

Increasing threats of radiological weapons have revitalized the researches for low cost large volume ?-ray and neutron ray sensors In the past few years we have designed and grown ternary and quaternary lead and thallium chalcogenides and lead selenoiodides for detectors to meet these challenges. These materials are congruent, can be tailored to enhance the parameters required for radiation sensors. In addition, this class of compounds can be grown by Bridgman method which promises for large volume productions. We have single crystals of several compounds from the melt including Tl3AsSe3, Tl3AsSe3-xSx, TlGaSe2, AgGaGe3Se8, AgxLi1-xAgGaGe3Se8 and PbTlI5-x Sex compounds. Experimental studies indicate that these have very low absorption coefficient, low defect density and can be fabricated in any shape and sizes. These crystals do not require post growth annealing and do not show any second phase precipitates when processed for electrode bonding and other fabrication steps. In this paper we report purification, growth and fabrication of large Tl3AsSe3 (TAS) crystals. We observed that TAS crystals grown by using further purification of as supplied high purity source materials followed by directionally solidified charge showed higher resistivity than previously reported values. TAS also showed constant value as the function of voltage. A low thermal gradient and high purity source material were used to reduce thermal stresses in large crystals. By improving the purification of the as supplied source materials very high quality thallium, selenium and arsenic was achieved for preparing stoichiometric Tl3AsSe3 compound. Low gradient (<20K/cm) and slow growth rate (1-2 cm/day) produced crystals with reduced stress. Crystals did not show any micro cracking during fabrication of crystals grown with high purity and at low thermal gradient. Since thallium is a major component and very sensitive to surface oxidation, removal of surface and bulk oxides is very important. Intentional increase in the growth rate from 1cm/day to higher speed (>5cm/day) showed very different morphologies on the surface of the crystals. Electrical resistivity was one order of magnitude higher than previously reported value and it was observed to be constant as the function of frequency.

The accumulation of two neolignan in the leaves, stems, and flower of red betel (Piper crocatum Ruiz & Pav.)

NASA Astrophysics Data System (ADS)

Hartini, Y. S.; Nugroho, L.

2017-05-01

Organ for the biosynthesis of secondary metabolite is not always a place for its biosynthesis, even the same compound was synthesized in the different organs in different plants. Neolignan is a secondary metabolite, known as an imunostimulant, synthesized through shikimic acid pathway with the important precursor is chorismic acid. The compound was known to be accumulated in the roots, stems and leaves of Piper regnellii with the concentration varies depending on the type of neolignan. It has been investigated the accumulation of two compound neolignans (Pc-1 and Pc-2) isolated from the methanol extract of red betel leaf (Piper crocatum Ruiz & Pav.) in the leaves, stems, and flowers of red betel. Chromatographic methods used was Gas Chromatography-Mass Spectrometry (GC-MS). Chromatogram of GC-MS showed that the Pc-1 with purity of 100%, m/z 460.3 could be detected at the minute of 29.986, while the Pc-2 with purity of 96.681%, m/z 418.3 was detected at the minute of 29.495. The research was then continued to investigate the existence and accumulation of both compounds in leaves, stems, and flowers of red betel. The GC-MS chromatogram shows that Pc-1 and Pc-2 could be detected in the leaves, stem and flower with various concentration among plant organs. Moreover, leaves contained the highest concentration of Pc-1 and Pc-2 compared to other plant organs.

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

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.

Synthesis of new 2,5-disubstituted-1,3,4-thiadiazole derivatives and their in vivo anticonvulsant activity.

PubMed

Harish, K P; Mohana, K N; Mallesha, L

2014-01-01

A series of 2,5-disubstituted-1,3,4-thiadiazole derivatives were synthesized by the reaction of 3-(2-cyanopropan-2-yl)-N-(5-(piperazine-1-yl)-1,3,4-thiadiazol-2-yl)benzamide with various sulfonyl chlorides and evaluated for their anticonvulsant activity in MES test. Rotorod method was employed to determine the neurotoxicity. The purity of the compounds is confirmed on the basis of their elemental analysis. The structures of all the new compounds are established on the basis of 1H NMR and mass spectral data. Out of fifteen compounds, three were found to be potent anticolvunstants. The same compounds showed no neurotoxicity at the maximum dose administered (100 mg/kg).

Experimental investigation of the ionization mechanisms of uranium in thermal ionization mass spectrometry in the presence of carbon

NASA Astrophysics Data System (ADS)

Kraiem, M.; Mayer, K.; Gouder, T.; Seibert, A.; Wiss, T.; Thiele, H.; Hiernaut, J.-P.

2010-01-01

Thermal ionization mass spectrometry (TIMS) is a well established instrumental technique for providing accurate and precise isotope ratio measurements of elements with reasonably low first ionization potential. In nuclear safeguards and in environmental research, it is often required to measure the isotope ratios in small samples of uranium. Empirical studies had shown that the ionization yield of uranium and plutonium in a TIMS ion source can be significantly increased in the presence of a carbon source. But, even though carbon appeared crucial in providing high ionization yields, processes taking place on the ionization surface were still not well understood. This paper describes the experimental results obtained from an extended study on the evaporation and ionization mechanisms of uranium occurring on a rhenium mass spectrometry filament in the presence of carbon. Solid state reactions were investigated using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Additionally, vaporization measurements were performed with a modified-Knudsen cell mass spectrometer for providing information on the neutral uranium species in the vapor phase. Upon heating, under vacuum, the uranyl nitrate sample was found to turn into a uranium carbide compound, independent of the type of carbon used as ionization enhancer. With further heating, uranium carbide leads to formation of single charged uranium metal ions and a small amount of uranium carbide ions. The results are relevant for a thorough understanding of the ion source chemistry of a uranyl nitrate sample under reducing conditions. The significant increase in ionization yield described by many authors on the basis of empirical results can be now fully explained and understood.

Passivation of uranium towards air corrosion by N 2+ and C + ion implantation

NASA Astrophysics Data System (ADS)

Arkush, R.; Mintz, M. H.; Shamir, N.

2000-10-01

The passivation of uranium surfaces against air corrosion, by ion implantation processes was studied, using surface analysis methods. Implanting 45 keV N +2 and C + ions produces thin modified surface layers with gradual gradients of the corresponding compounds (i.e., nitrides and carbides, respectively), which avoid the formation of discontinuous interfaces typical to coatings. Such gradual interfaces impart excellent mechanical stability and adhesion to the modified layers, in spite of the large misfit between the metal substrate and the implantation on induced compounds. It turns out that these layers provide an almost absolute protection against air corrosion. A rapid initial stage of oxidation of the modified surface layers takes place, forming very thin protective oxidation zones (1-4 nm thick), which practically stop further air oxidation for years. The mechanism of the initial oxidation stage of the modified layers seems to vary with the type of surface (i.e., either nitrides or carbides). However, in any case the protection ability of the formed oxidation products is excellent, probably due to the close match between these compounds and the underlying nitrides or carbides.

Pseudopotential for ab initio calculations of uranium compounds

NASA Astrophysics Data System (ADS)

Smirnov, G. S.; Pisarev, V. V.; Stegailov, V. V.

2018-01-01

The density functional theory (DFT) is a research tool of the highest importance for electronic structure calculations. It is often the only affordable method for ab initio calculations of complex materials. The pseudopotential approach allows reducing the total number of electrons in the model that speeds up calculations. However, there is a lack of pseudopotentials for heavy elements suitable for condensed matter DFT models. In this work, we present a pseudopotential for uranium developed in the Goedecker-Teter-Hutter form. Its accuracy is illustrated using several molecular and solid-state calculations.

METHOD FOR THE RECOVERY AND PURIFICATION OF GASEOUS UF$sub 6$ FROM GASEOUS MIXTURES AND UF$sub 7$NO AND UF$sub 7$NO$sub 2$ PRODUCTS PRODUCED THEREBY

DOEpatents

Ogle, P.R. Jr.

1962-06-16

A method is given for recovering uranium hexafluoride from a gaseous mixture containing said uranium hexafluoride and extraneous gaseous impurities. The method comprises reacting said mixture with a nitrogen oxyfluoride at a temperature in the range - 100 to 50 deg C to thereby form a solid compound having the empirical formula UF/sub 7/N(O)/sub x/ where x is a number from 1 to 2. (AEC)

Formation of unprecedented actinidecarbon triple bonds in uranium methylidyne molecules

PubMed Central

Lyon, Jonathan T.; Hu, Han-Shi; Andrews, Lester; Li, Jun

2007-01-01

Chemistry of the actinide elements represents a challenging yet vital scientific frontier. Development of actinide chemistry requires fundamental understanding of the relative roles of actinide valence-region orbitals and the nature of their chemical bonding. We report here an experimental and theoretical investigation of the uranium methylidyne molecules X3UCH (X = F, Cl, Br), F2ClUCH, and F3UCF formed through reactions of laser-ablated uranium atoms and trihalomethanes or carbon tetrafluoride in excess argon. By using matrix infrared spectroscopy and relativistic quantum chemistry calculations, we have shown that these actinide complexes possess relatively strong UC triple bonds between the U 6d-5f hybrid orbitals and carbon 2s-2p orbitals. Electron-withdrawing ligands are critical in stabilizing the U(VI) oxidation state and sustaining the formation of uranium multiple bonds. These unique UC-bearing molecules are examples of the long-sought actinide-alkylidynes. This discovery opens the door to the rational synthesis of triple-bonded actinidecarbon compounds. PMID:18024591

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.

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

PubMed

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

2018-03-01

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

Compared in vivo efficiency of nanoemulsions unloaded and loaded with calixarene and soapy water in the treatment of superficial wounds contaminated by uranium.

PubMed

Grivès, Sophie; Phan, Guillaume; Bouvier-Capely, Céline; Suhard, David; Rebière, François; Agarande, Michelle; Fattal, Elias

2017-04-01

No emergency decontamination treatment is currently available in the case of radiological skin contamination by uranium compounds. First responders in the workplace or during an industrial nuclear accident must be able to treat internal contamination through skin. For this purpose, a calixarene nanoemulsion was developed for the treatment of intact skin or superficial wounds contaminated by uranium, and the decontamination efficiency of this nanoemulsion was investigated in vitro and ex vivo. The present work addresses the in vivo decontamination efficiency of this nanoemulsion, using a rat model. This efficiency is compared to the radio-decontaminant soapy water currently used in France (Trait rouge ® ) in the workplace. The results showed that both calixarene-loaded nanoemulsion and non-loaded nanoemulsion allowed a significant decontamination efficiency compared to the treatment with soapy water. Early application of the nanoemulsions on contaminated excoriated rat skin allowed decreasing the uranium content by around 85% in femurs, 95% in kidneys and 93% in urines. For skin wounded by microneedles, mimicking wounds by microstings, nanoemulsions allowed approximately a 94% decrease in the uranium retention in kidneys. However, specific chelation of uranium by calixarene molecules within the nanoemulsion was not statistically significant, probably because of the limited calixarene-to-uranium molar ratio in these experiment conditions. Moreover, these studies showed that the soapy water treatment potentiates the transcutaneous passage of uranium, thus making it bioavailable, in particular when the skin is superficially wounded. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Uranium series isotopes concentration in sediments at San Marcos and Luis L. Leon reservoirs, Chihuahua, Mexico

NASA Astrophysics Data System (ADS)

Méndez-García, C.; Renteria-Villalobos, M.; García-Tenorio, R.; Montero-Cabrera, M. E.

2014-07-01

Spatial and temporal distribution of the radioisotopes concentrations were determined in sediments near the surface and core samples extracted from two reservoirs located in an arid region close to Chihuahua City, Mexico. At San Marcos reservoir one core was studied, while from Luis L. Leon reservoir one core from the entrance and another one close to the wall were investigated. 232Th-series, 238U-series, 40K and 137Cs activity concentrations (AC, Bq kg-1) were determined by gamma spectrometry with a high purity Ge detector. 238U and 234U ACs were obtained by liquid scintillation and alpha spectrometry with a surface barrier detector. Dating of core sediments was performed applying CRS method to 210Pb activities. Results were verified by 137Cs AC. Resulting activity concentrations were compared among corresponding surface and core sediments. High 238U-series AC values were found in sediments from San Marcos reservoir, because this site is located close to the Victorino uranium deposit. Low AC values found in Luis L. Leon reservoir suggest that the uranium present in the source of the Sacramento - Chuviscar Rivers is not transported up to the Conchos River. Activity ratios (AR) 234U/overflow="scroll">238U and 238U/overflow="scroll">226Ra in sediments have values between 0.9-1.2, showing a behavior close to radioactive equilibrium in the entire basin. 232Th/overflow="scroll">238U, 228Ra/overflow="scroll">226Ra ARs are witnesses of the different geological origin of sediments from San Marcos and Luis L. Leon reservoirs.

Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.

DOE PAGES

Pagano, Justin Kane; Scott, Brian Lindley; Kiplinger, Jaqueline Loetsch

2018-06-09

Two new uranium metallacyclopropenes, (C 5Me 4R) 2U(η 2-Ph 2PC=CPPh 2) (R = Me, Et) were prepared by reducing the corresponding (C 5Me 4R) 2UCl 2 complexes with KC 8 in the presence of 1,2-bis(diphenylphosphino)acetylene (Ph 2P–C≡C–PPh 2). Both compounds were fully characterized by a combination of elemental analysis and multinuclear NMR, UV–visible–NIR, and IR spectroscopies. Differences in the electronic spectra of these novel compounds and the known (C 5Me 5) 2U(η 2-Me 3SiC=CSiMe 3) are discussed. Finally, also presented is the solid-state structure of (C 5Me 4Et) 2U(η 2-Ph 2PC=CPPh 2), which reveals significant distortions of the coordinated 1,2-bis(diphenylphosphino)acetylenemore » (Ph 2P–C≡C–PPh 2) ligand.« less

Synthesis, characterization, and reactivity of the first uranium metallocene 1,2 bis(diphenylphosphino)acetylene complexes.

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

Pagano, Justin Kane; Scott, Brian Lindley; Kiplinger, Jaqueline Loetsch

Two new uranium metallacyclopropenes, (C 5Me 4R) 2U(η 2-Ph 2PC=CPPh 2) (R = Me, Et) were prepared by reducing the corresponding (C 5Me 4R) 2UCl 2 complexes with KC 8 in the presence of 1,2-bis(diphenylphosphino)acetylene (Ph 2P–C≡C–PPh 2). Both compounds were fully characterized by a combination of elemental analysis and multinuclear NMR, UV–visible–NIR, and IR spectroscopies. Differences in the electronic spectra of these novel compounds and the known (C 5Me 5) 2U(η 2-Me 3SiC=CSiMe 3) are discussed. Finally, also presented is the solid-state structure of (C 5Me 4Et) 2U(η 2-Ph 2PC=CPPh 2), which reveals significant distortions of the coordinated 1,2-bis(diphenylphosphino)acetylenemore » (Ph 2P–C≡C–PPh 2) ligand.« less

Germanium and uranium in coalified wood bom upper Devonian black shale

USGS Publications Warehouse

Breger, I.A.; Schopf, J.M.

1955-01-01

Microscopic study of black, vitreous, carbonaceous material occurring in the Chattanooga shale in Tennessee and in the Cleveland member of the Ohio shale in Ohio has revealed coalified woody plant tissue. Some samples have shown sufficient detail to be identified with the genus Cauixylon. Similar material has been reported in the literature as "bituminous" or "asphaltic" stringers. Spectrographic analyses of the ash from the coalified wood have shown unusually high percentages of germanium, uranium, vanadium, and nickel. The inverse relationship between uranium and germanium in the ash and the ash content of various samples shows an association of these elements with the organic constituents of the coal. On the basis of geochemical considerations, it seems most probable that the wood or coalified wood was germanium-bearing at the time logs or woody fragmenta were floated into the basins of deposition of the Chattanooga shale and the Cleveland member of the Ohio shale. Once within the marine environment, the material probably absorbed uranium with the formation of organo-uranium compounds such as exist in coals. It is suggested that a more systematic search for germaniferous coals in the vicinity of the Chattanooga shale and the Cleveland member of the Ohio shale might be rewarding. ?? 1955.

Anti-prelog reduction of prochiral carbonyl compounds by Oenococcus oeni in a biphasic system.

PubMed

Hu, Jian; Xu, Yan

2006-07-01

An aqueous-organic biphasic system was established and used with whole cells of Oenococcus oeni to reduce 2-octanone to (R)-2-octanol. The conversion reached 99% when the Tris/borate buffer was increased from 50 mM to 300 mM in the aqueous phase. In addition, the conversion increased as the log P value of the organic solvent changed from 0.5 to 6.6. Under optimized conditions, the conversion of (R)-2-octanol reached 99% from 0.5 M 2-octanone with an optical purity of 99% e.e. The biphasic system allows the anti-Prelog reduction of aliphatic and aromatic ketones to furnish (R)-configurated alcohols in high optical purity as well.

Synthesis, crystal structure and redox properties of dihydropyrazole-bridged ferrocene-based derivatives

NASA Astrophysics Data System (ADS)

Li, Heng-Dong; Ma, Zai-He; Yang, Kun; Xie, Li-Li; Yuan, Yao-Feng

2012-09-01

Dihydropyrazole-bridged ferrocene-based derivatives were prepared by corresponding chalcones with hydrazine hydrate, then acylation with 3-(ethoxycarbonyl)propionyl chloride directly in high yields and purity. All of these compounds were characterized by MS, IR, 1H NMR, 13C NMR and elemental analysis. The relationship between the structure and redox properties was investigated based on the results of single crystal X-ray structure determinations and cyclic voltammetry. The mechanism of the electron transfer for representative compound 4b was verified by density functional theory (DFT) calculations.

Containerless automated processing of intermetallic compounds and composites

NASA Technical Reports Server (NTRS)

Johnson, D. R.; Joslin, S. M.; Reviere, R. D.; Oliver, B. F.; Noebe, R. D.

1993-01-01

An automated containerless processing system has been developed to directionally solidify high temperature materials, intermetallic compounds, and intermetallic/metallic composites. The system incorporates a wide range of ultra-high purity chemical processing conditions. The utilization of image processing for automated control negates the need for temperature measurements for process control. The list of recent systems that have been processed includes Cr, Mo, Mn, Nb, Ni, Ti, V, and Zr containing aluminides. Possible uses of the system, process control approaches, and properties and structures of recently processed intermetallics are reviewed.

PREPARATION OF PURE METAL FROM THEIR COMPOUNDS

DOEpatents

Slatin, H.L.

1961-08-01

S>A method is described for the preparation of uranium from U/sub 3/O/ sub 6/ by electrolytic deposition at the cathode from an alkali and/or alkaline earth fused salt bath such as fused strontium potassium chloride. (AEC)

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.

Preparation of polyurethane foams using fractionated products in liquefied wood

Treesearch

Junming Xu; Jianchun Jiang; Chung-Yun Hse; Todd F. Shupe

2014-01-01

Liquefaction of sawdust was studied using glycerol and methanol as mix solvents. A new bio-polyol product consisting of high purity multi-hydroxy compounds was obtained by precipitation of the hydrophobic organics from the liquefied product in an aqueous solution. As identified by GC-MS, the dominate components in bio-polyol were glycerol, glycerol derivatives, and...

TC-99 Decontaminant from heat treated gaseous diffusion membrane -Phase I, Part B

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

Oji, L.; Restivo, M.; Duignan, M.

2017-11-01

Uranium gaseous diffusion cascades represent a significant environmental challenge to dismantle, containerize and dispose as low-level radioactive waste. Baseline technologies rely on manual manipulations involving direct access to technetium-contaminated piping and materials. There is a potential to utilize novel decontamination technologies to remove the technetium and allow for on-site disposal of the very large uranium converters. Technetium entered these gaseous diffusion cascades as a hexafluoride complex in the same fashion as uranium. Technetium, as the isotope Tc-99, is an impurity that follows uranium in the first cycle of the Plutonium and Uranium Extraction (PUREX) process. The technetium speciation or exactmore » form in the gaseous diffusion cascades is not well defined. Several forms of Tc-99 compounds, mostly the fluorinated technetium compounds with varying degrees of volatility have been speculated by the scientific community to be present in these cascades. Therefore, there may be a possibility of using thermal or leaching desorption, which is independent of the technetium oxidation states, to perform an insitu removal of the technetium as a volatile species and trap the radionuclide on sorbent traps which could be disposed as low-level waste. Based on the positive results of the first part of this work1 the use of steam as a thermal decontamination agent was further explored with a second piece of used barrier material from a different location. This new series of tests included exposing more of the material surface to the flow of high temperature steam through the change in the reactor design, subjecting it to alternating periods of stream and vacuum, as well as determining if a lower temperature steam, i.e., 121°C (250°F) would be effective, too. Along with these methods, one other simpler method involving the leaching of the Tc-99 contaminated barrier material with a 1.0 M aqueous solution of ammonium carbonate, with and without sonication, was evaluated.« less

Mineral resources of the Raymond Mountain Wilderness Study Area, Lincoln county, Wyoming

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

Lund, K.; Evans, J.P.; Hill, R.H.

1990-01-01

The paper reports on the Raymond Mountain Wilderness Study Area which encompasses most of the Sublette Range of western Lincoln County, Wyo. The study area consists of upper Paleozoic and Mesozoic sedimentary rocks that form part of the Idaho-Wyoming-Utah overthrust belt. There are no identified mineral or energy resources in the wilderness study area. The study area has moderate energy resource potential for oil and gas. Mineral resource potential for vanadium and phosphate is low because the Phosphoria Formation is deeply buried beneath the wilderness study area and contains unweathered units having low P{sub 2}O{sub 5} values. The mineral resourcemore » potential for coal, other metals, including uranium, high-purity limestone or dolostone, and geothermal energy is low.« less

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

Voorhees, D.R.; Rossmassler, R.L.; Zimmer, G.

The tritium analytical system at TFTR is used to determine the purity of tritium bearing gas streams in order to provide inventory and accountability measurements. The system includes a quadrupole mass spectrometer (QMS) and beta scintillator originally configured at Monsanto Mound Research Laboratory. The system was commissioned and tested in 1992 and is used daily for analysis of calibration standards, incoming tritium shipments, gases evolved from uranium storage beds and effluent gases from the tokamak. The instruments are controlled by a personal computer with customized software written with a graphical programming system designed for data acquisition and control. A discussionmore » of the instrumentation, control systems, system parameters, procedural methods, algorithms, and operational issues will be presented. Measurements of gas holding tanks and tritiated water waste streams using ion chamber instrumentation are discussed elsewhere. 7 refs., 3 figs.« less

PURIFICATION PROCESS

DOEpatents

Wibbles, H.L.; Miller, E.I.

1958-01-14

This patent deals with the separation of uranium from molybdenum compounds, and in particular with their separation from ether solutions containing the molybdenum in the form of acids, such as silicomolybdic and phosphomolybdic acids. After the nitric acid leach of pitchblende, the molybdenum values present in the ore are found in the leach solution in the form of complex acids. The uranium bearing solution may be purified of this molybdenum content by comtacting it with activated charcoal. The purification is improved when the acidity of the solution is low ad agitation is also beneficial. The molybdenum may subsequently be recovered from the charcosl ad the charcoal reused.

Scanning Transmission Electron Microscopy at High Resolution

PubMed Central

Wall, J.; Langmore, J.; Isaacson, M.; Crewe, A. V.

1974-01-01

We have shown that a scanning transmission electron microscope with a high brightness field emission source is capable of obtaining better than 3 Å resolution using 30 to 40 keV electrons. Elastic dark field images of single atoms of uranium and mercury are shown which demonstrate this fact as determined by a modified Rayleigh criterion. Point-to-point micrograph resolution between 2.5 and 3.0 Å is found in dark field images of micro-crystallites of uranium and thorium compounds. Furthermore, adequate contrast is available to observe single atoms as light as silver. Images PMID:4521050

SEPARATION PROCESS USING COMPLEXING AND ADSORPTION

DOEpatents

Spedding, J.H.; Ayers, J.A.

1958-06-01

An adsorption process is described for separating plutonium from a solution of neutron-irradiated uranium containing ions of a compound of plutonium and other cations. The method consists of forming a chelate complex compound with plutoniunn ions in the solution by adding a derivative of 8- hydroxyquinoline, which derivative contains a sulfonic acid group, and adsorbing the remaining cations from the solution on a cation exchange resin, while the complexed plutonium remains in the solution.

Method for the simultaneous preparation of radon-211, xenon-125, xenon-123, astatine-211, iodine-125 and iodine-123

DOEpatents

Mirzadeh, S.; Lambrecht, R.M.

1985-07-01

The invention relates to a practical method for commercially producing radiopharmaceutical activities and, more particularly, relates to a method for the preparation of about equal amount of Radon-211 (/sup 211/Rn) and Xenon-125 (/sup 125/Xe) including a one-step chemical procedure following an irradiation procedure in which a selected target of Thorium (/sup 232/Th) or Uranium (/sup 238/U) is irradiated. The disclosed method is also effective for the preparation in a one-step chemical procedure of substantially equal amounts of high purity /sup 123/I and /sup 211/At. In one preferred arrangement of the invention almost equal quantities of /sup 211/Rn and /sup 125/Xe are prepared using a onestep chemical procedure in which a suitably irradiated fertile target material, such as thorium-232 or uranium-238, is treated to extract those radionuclides from it. In the same one-step chemical procedure about equal quantities of /sup 211/At and /sup 123/I are prepared and stored for subsequent use. In a modified arrangement of the method of the invention, it is practiced to separate and store about equal amounts of only /sup 211/Rn and /sup 125/Xe, while preventing the extraction or storage of the radionuclides /sup 211/At and /sup 123/I.

Summary of ORSphere critical and reactor physics measurements

NASA Astrophysics Data System (ADS)

Marshall, Margaret A.; Bess, John D.

2017-09-01

In the early 1970s Dr. John T. Mihalczo (team leader), J.J. Lynn, and J.R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950s. The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared with the GODIVA I experiments. This critical configuration has been evaluated. Preliminary results were presented at ND2013. Since then, the evaluation was finalized and judged to be an acceptable benchmark experiment for the International Criticality Safety Benchmark Experiment Project (ICSBEP). Additionally, reactor physics measurements were performed to determine surface button worths, central void worth, delayed neutron fraction, prompt neutron decay constant, fission density and neutron importance. These measurements have been evaluated and found to be acceptable experiments and are discussed in full detail in the International Handbook of Evaluated Reactor Physics Benchmark Experiments. The purpose of this paper is to summarize all the evaluated critical and reactor physics measurements evaluations.

Experimental thermochemistry of neptunium oxides: Np2O5 and NpO2

NASA Astrophysics Data System (ADS)

Zhang, Lei; Dzik, Ewa A.; Sigmon, Ginger E.; Szymanowski, Jennifer E. S.; Navrotsky, Alexandra; Burns, Peter C.

2018-04-01

Neptunium (Np) compounds are important in the nuclear fuel cycle because of the buildup and long half-life (2.14 Ma) of Np-237 in nuclear waste, especially during long-term disposal in a geological repository. Neptunium in environmental conditions exists mainly in two oxidation states (+5 and + 4) and can substitute for uranium and/or rare earths in solid phases. Yet thermochemical data for solid neptunium compounds are scarce, despite being critical for evaluating the environmental transport of this radioactive and toxic element. Although high temperature oxide melt solution calorimetry has proven very useful in obtaining thermodynamic data for the formation of uranium and thorium oxide materials, it has not yet been applied to transuranium compounds. Continuing a program at Notre Dame to study the thermodynamics of transuranium compounds, we report the first determination of the enthalpies of drop solution of well-characterized neptunium oxides (Np2O5 and NpO2) using oxide melt solution calorimetry in molten sodium molybdate solvent at 973 K. The enthalpy of the decomposition reaction, Np2O5(cr) = 2NpO2(cr) + 1/2O2(g) at 298 K, is determined to be 7.70 ± 5.86 kJ/mol, and this direct measurement is consistent with existing thermodynamic data. The calorimetric methodology is straightforward and produces reliable data using milligram quantities of radioactive materials, and can be applied to many other transuranium compounds.

One-pot microwave assisted synthesis and structural elucidation of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates with larvicidal activity against Anopheles arabiensis

NASA Astrophysics Data System (ADS)

Chandrashekharappa, Sandeep; Venugopala, Katharigatta N.; Nayak, Susanta K.; Gleiser, Raquel M.; García, Daniel A.; Kumalo, Hezekiel M.; Kulkarni, Rashmi S.; Mahomoodally, Fawzi M.; Venugopala, Rashmi; Mohan, Mahendra K.; Odhav, Bharti

2018-03-01

In the present investigation a series of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates was achieved by microwave assisted one-pot method. The purity of the compounds was ascertained by HPLC and structural elucidation of the title compounds was achieved by FT-IR, NMR (1H and 13C), LC-MS and elemental analysis. One randomly selected compound from the series was further studied by single crystal X-ray method for intra and intermolecular interactions. Larvicidal properties of the characterized compounds were evaluated against Anopheles arabiensis and it was found that indolizine pharmacophore influences larvicidal activity as we can see larvicidal activity for all the analogues. The synthesized analogues (2j, 2m and 2f) were the most potent compounds based on the functional groups on the indolizine pharmacophore for larvicidal assay.

Performance Indicators for Uranium Bioremediation in the Subsurface: Basis and Assessment

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

Long, Philip E.; Yabusaki, Steven B.

2006-12-29

The purpose of this letter report is to identify performance indicators for in situ engineered bioremediation of subsurface uranium (U) contamination. This report focuses on in situ treatment of groundwater by biostimulation of extant in situ microbial populations (see http://128.3.7.51/NABIR/generalinfo/primers_guides/03_NABIR_primer.pdf for background information on bioremediation of metals and radionuclides). The treatment process involves amendment of the subsurface with an electron donor such as acetate, lactate, ethanol or other organic compound such that in situ microorganisms mediate the reduction of U(VI) to U(IV). U(VI) precipitates as uraninite or other insoluble U phase. Uranium is thus immobilized in place by such processesmore » and is subject to reoxidation that may remobilize the reduced uranium. Related processes include augmenting the extant subsurface microbial populations, addition of electron acceptors, and introduction of chemically reducing materials such as zero-valent Fe. While metrics for such processes may be similar to those for in situ biostimulation, these related processes are not directly in the scope of this letter report.« less

Germanium and uranium in coalified wood from Upper Devonian black shale

USGS Publications Warehouse

Breger, Irving A.; Schopf, James M.

1954-01-01

Microscopic study of black, vitreous, carbonaceous material occurring in the Chattanooga shale in Tennessee and in the Cleveland member of the Ohio shale in Ohio has revealed coalified woody plant tissue. Some samples have shown sufficient detail to be identified with the genus Callixylon. Similar material has been reported in the literature as "bituminous" or "asphaltic" stringers. Spectrographic analyses of the ash from the coalified wood have shown unusually high percentages of germanium, uranium, vanadium, and nickel. The inverse relationship between uranium and germanium in the ash and the ash content of various samples shows an association of these elements with the organic constituents of the coal. On the basis of geochemical considerations, it seems most probable that the wood or coalified wood was germanium-bearing at the time logs or woody fragments were floated into the basins of deposition of the Chattanooga shale and the Cleveland member of the Ohio shale. Once within the marine environment, the material probably absorbed uranium with the formation of organo-uranium compounds such as have been found to exist in coals. It is suggested that a more systematic search for germaniferous coals in the vicinity of the Chattanooga shale and the Cleveland member of the Ohio shale might be rewarding.

Unraveling uranium induced oxidative stress related responses in Arabidopsis thaliana seedlings. Part II: responses in the leaves and general conclusions.

PubMed

Vanhoudt, Nathalie; Cuypers, Ann; Horemans, Nele; Remans, Tony; Opdenakker, Kelly; Smeets, Karen; Bello, Daniel Martinez; Havaux, Michel; Wannijn, Jean; Van Hees, May; Vangronsveld, Jaco; Vandenhove, Hildegarde

2011-06-01

The cellular redox balance seems an important modulator under heavy metal stress. While for other heavy metals these processes are well studied, oxidative stress related responses are also known to be triggered under uranium stress but information remains limited. This study aimed to further unravel the mechanisms by which plants respond to uranium stress. Seventeen-day-old Arabidopsis thaliana seedlings, grown on a modified Hoagland solution under controlled conditions, were exposed to 0, 0.1, 1, 10 and 100 μM uranium for 1, 3 and 7 days. While in Part I of this study oxidative stress related responses in the roots were discussed, this second Part II discusses oxidative stress related responses in the leaves and general conclusions drawn from the results of the roots and the leaves will be presented. As several responses were already visible following 1 day exposure, when uranium concentrations in the leaves were negligible, a root-to-shoot signaling system was suggested in which plastids could be important sensing sites. While lipid peroxidation, based on the amount of thiobarbituric acid reactive compounds, was observed after exposure to 100 μM uranium, affecting membrane structure and function, a transient concentration dependent response pattern was visible for lipoxygenase initiated lipid peroxidation. This transient character of uranium stress responses in leaves was emphasized by results of lipoxygenase (LOX2) and antioxidative enzyme transcript levels, enzyme capacities and glutathione concentrations both in time as with concentration. The ascorbate redox balance seemed an important modulator of uranium stress responses in the leaves as in addition to the previous transient responses, the total ascorbate concentration and ascorbate/dehydroascorbate redox balance increased in a concentration and time dependent manner. This could represent either a slow transient response or a stable increase with regard to plant acclimation to uranium stress. Copyright © 2011 Elsevier Ltd. All rights reserved.

Uranium series isotopes concentration in sediments at San Marcos and Luis L. Leon reservoirs, Chihuahua, Mexico

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

Méndez-García, C.; Montero-Cabrera, M. E., E-mail: elena.montero@cimav.edu.mx; Renteria-Villalobos, M.

2008-01-01

Spatial and temporal distribution of the radioisotopes concentrations were determined in sediments near the surface and core samples extracted from two reservoirs located in an arid region close to Chihuahua City, Mexico. At San Marcos reservoir one core was studied, while from Luis L. Leon reservoir one core from the entrance and another one close to the wall were investigated. ²³²Th-series, ²³⁸U-series, ⁴⁰K and ¹³⁷Cs activity concentrations (AC, Bq kg⁻¹) were determined by gamma spectrometry with a high purity Ge detector. ²³⁸U and ²³⁴U ACs were obtained by liquid scintillation and alpha spectrometry with a surface barrier detector. Dating ofmore » core sediments was performed applying CRS method to ²¹⁰Pb activities. Results were verified by ¹³⁷Cs AC. Resulting activity concentrations were compared among corresponding surface and core sediments. High ²³⁸U-series AC values were found in sediments from San Marcos reservoir, because this site is located close to the Victorino uranium deposit. Low AC values found in Luis L. Leon reservoir suggest that the uranium present in the source of the Sacramento – Chuviscar Rivers is not transported up to the Conchos River. Activity ratios (AR) ²³⁴U/²³⁸U and ²³⁸U/²²⁶Ra in sediments have values between 0.9–1.2, showing a behavior close to radioactive equilibrium in the entire basin. ²³²Th/²³⁸U, ²²⁸Ra/²²⁶Ra ARs are witnesses of the different geological origin of sediments from San Marcos and Luis L. Leon reservoirs.« less

Preparative purification of the major anti-inflammatory triterpenoid esters from Marigold (Calendula officinalis).

PubMed

Hamburger, M; Adler, S; Baumann, D; Förg, A; Weinreich, B

2003-06-01

A method for the efficient preparative purification of faradiol 3-O-laurate, palmitate and myristate, the major anti-inflammatory triterpenoid esters in the flower heads of the medicinal plant Calendula officinalis has been developed. Gram quantities of the individual compounds were obtained with 96 to 98% purity by a combination of supercritical fluid extraction (SFE), normal-phase and reversed-phase column chromatography. During the work-up of the faradiol esters, accompanying minor compounds of the triterpene ester fraction were purified and identified by spectroscopic means as maniladiol 3-O-laurate and myristate.

Contamination Analyzer

NASA Technical Reports Server (NTRS)

1994-01-01

Measurement of the total organic carbon content in water is important in assessing contamination levels in high purity water for power generation, pharmaceutical production and electronics manufacture. Even trace levels of organic compounds can cause defects in manufactured products. The Sievers Model 800 Total Organic Carbon (TOC) Analyzer, based on technology developed for the Space Station, uses a strong chemical oxidizing agent and ultraviolet light to convert organic compounds in water to carbon dioxide. After ionizing the carbon dioxide, the amount of ions is determined by measuring the conductivity of the deionized water. The new technique is highly sensitive, does not require compressed gas, and maintenance is minimal.

The control of purity and stoichiometry of compound semiconductors by high vapor pressure transport

NASA Technical Reports Server (NTRS)

Bachmann, Klaus J.; Ito, Kazufumi; Scroggs, Jeffery S.; Tran, Hien T.

1995-01-01

In this report we summarize the results of a three year research program on high pressure vapor transport (HPVT) of compound semiconductors. Most of our work focused onto pnictides, in particular ZnGeP2, as a model system. Access to single crystals of well controlled composition of this material is desired for advancing the understanding and control of its point defect chemistry in the contest of remote, real-time sensing of trace impurities, e.g., greenhouse gases, in the atmosphere by ZnGeP2 optical parametric oscillators (OPO's).

29 CFR 1926.55 - Gases, vapors, fumes, dusts, and mists.

Code of Federal Regulations, 2013 CFR

2013-07-01

... Nitrous oxide 10024-97-2 E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist... — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist Total dust — — Respirable...

29 CFR 1926.55 - Gases, vapors, fumes, dusts, and mists.

Code of Federal Regulations, 2014 CFR

2014-07-01

... Nitrous oxide 10024-97-2 E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist... — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist Total dust — — Respirable...

29 CFR 1915.1000 - Air contaminants.

Code of Federal Regulations, 2012 CFR

2012-07-01

... E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist, mineral 8012-95-1 — 5... — Turpentine 8006-64-2 100 560 — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist...

29 CFR 1915.1000 - Air contaminants.

Code of Federal Regulations, 2014 CFR

2014-07-01

... E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist, mineral 8012-95-1 — 5... — Turpentine 8006-64-2 100 560 — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist...

29 CFR 1926.55 - Gases, vapors, fumes, dusts, and mists.

Code of Federal Regulations, 2012 CFR

2012-07-01

... Nitrous oxide 10024-97-2 E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist... — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist Total dust — — Respirable...

29 CFR 1915.1000 - Air contaminants.

Code of Federal Regulations, 2013 CFR

2013-07-01

... E Octachloronaphthalene 2234-13-1 — 0.1 X Octane 111-65-9 400 1900 — Oil mist, mineral 8012-95-1 — 5... — Turpentine 8006-64-2 100 560 — Uranium (as U) 7440-61-1 Soluble compounds — 0.2 — Insoluble compounds — 0.2 — Vanadium 1314-62-1 Respirable dust (as V2 O5) — (C)0.5 — Fume (as V2 O5) — (C)0.1 — Vegetable oil mist...

Electronic and Magnetic Structures, Magnetic Hyperfine Fields and Electric Field Gradients in UX3 (X = In, Tl, Pb) Intermetallic Compounds

NASA Astrophysics Data System (ADS)

Khan, Sajid; Yazdani-Kachoei, Majid; Jalali-Asadabadi, Saeid; Farooq, Muhammad Bilal; Ahmad, Iftikhar

2018-02-01

Cubic uranium compounds such as UX3 (X is a non-transition element of groups IIIA or IVA) exhibit highly diverse magnetic properties, including Pauli paramagnetism, spin fluctuation and anti-ferromagnetism. In the present paper, we explore the structural, electronic and magnetic properties as well as the hyperfine fields (HFFs) and electric field gradients (EFGs) with quadrupole coupling constant of UX3 (X = In, Tl, Pb) compounds using local density approximation, Perdew-Burke-Ernzerhof parametrization of generalized gradient approximation (PBE-GGA) including the Hubbard U parameter (GGA + U), a revised version of PBE-GGA that improves equilibrium properties of densely packed solids and their surfaces (PBEsol-GGA), and a hybrid functional (HF-PBEsol). The spin orbit-coupling calculations have been added to investigate the relativistic effect of electrons in these materials. The comparison between the experimental parameters and our calculated structural parameters we confirm the consistency and effectiveness of our theoretical tools. The computed magnetic moments show that magnetic moment increases from indium to lead in the UX3 family, and all these compounds are antiferromagnetic in nature. The EFGs and HFFs, as well as the quadrupole coupling constant of UX3 (X = In, Tl, Pb), are discussed in detail. These properties primarily originate from f and p states of uranium and post-transition sites.

Carbon-14 radiolabelling and tissue distribution evaluation of a potential anti-TB compound.

PubMed

Sonopo, Molahlehi S; Venter, Kobus; Winks, Susan; Marjanovic-Painter, Biljana; Morgans, Garreth L; Zeevaart, Jan R

2016-06-15

This paper describes a five-step synthesis of a carbon-14-labelled pyrazole compound (11). A total of 2.96 MBq of 11 was obtained with the specific activity of 2242.4 MBq/mmol. The radiochemical purity was >99%, and the overall radiochemical yield was 60% based on the [(14) C6 ] 4-bromoaniline starting material. Biodistribution results showed that the radiotracer (administrated orally) has a high accumulation in the small intestine, large intestine and liver of both non-infected and tuberculosis (TB)-infected mice. Therefore, this suggests that compound 11 undergoes hepatobiliary clearance. The compound under investigation has been found to be slowly released from the liver between 2 and 8 h. The study revealed that 11 has no affinity for TB cells. Copyright © 2016 John Wiley & Sons, Ltd.

Dielectric and impedance studies of Ba0.50(Na0.25Bi0.25)(Fe0.25Nb0.25)Ti0.50O3 ceramic

NASA Astrophysics Data System (ADS)

Yadav, Anjana; Chandra, K. P.; Kulkarni, A. R.; Prasad, K.

2018-05-01

Lead-free perovskite Ba0.50(Na0.25Bi0.25)(Fe0.25Nb0.25)Ti0.50O3 was prepared using conventional ceramic technique at 1130°C/4h in air atmosphere and characterized by X-ray diffraction, scanning electron microscopy, dielectric and impedance studies. XRD analysis of the compound indicated the formation of a single-phase cubic structure. SEM study was carried out to study the quality and purity of the compound. Compound showed very high dielectric constant (33700). Impedance analysis indicated the negative temperature coefficient of resistance character of the compound. Ac conductivity data followed Jonscher's law and correlated barrier hopping successfully explained the charge carrier transport mechanism in the system.

Monomers for thermosetting and toughening epoxy resins. [glycidyl amine derivatives, propargyl-containing amines, and mutagenic testing of aromatic diamines

NASA Technical Reports Server (NTRS)

Pratt, J. R.

1981-01-01

Eight glycidyl amines were prepared by alkylating the parent amine with epichlorohydrin to form chlorohydrin, followed by cyclization with aqueous NaOH. Three of these compounds contained propargyl groups with postcuring studies. A procedure for quantitatively estimating the epoxy content of these glycidyl amines was employed for purity determination. Two diamond carbonates and several model propargly compounds were prepared. The synthesis of three new diamines, two which contain propargyloxy groups, and another with a sec-butyl group is in progress. These materials are at the dinitro stage ready for the final hydrogenation step. Four aromatic diamines were synthesized for mutagenic testing purposes. One of these compounds rapidly decomposes on exposure to air.

Investigation of the electronic ground states for a reduced pyridine(diimine) uranium series: evidence for a ligand tetraanion stabilized by a uranium dimer.

PubMed

Anderson, Nickolas H; Odoh, Samuel O; Williams, Ursula J; Lewis, Andrew J; Wagner, Gregory L; Lezama Pacheco, Juan; Kozimor, Stosh A; Gagliardi, Laura; Schelter, Eric J; Bart, Suzanne C

2015-04-15

The electronic structures of a series of highly reduced uranium complexes bearing the redox-active pyridine(diimine) ligand, (Mes)PDI(Me) ((Mes)PDI(Me) = 2,6-(2,4,6-Me3-C6H2-N═CMe)2C5H3N) have been investigated. The complexes, ((Mes)PDI(Me))UI3(THF) (1), ((Mes)PDI(Me))UI2(THF)2 (2), [((Mes)PDI(Me))UI]2 (3), and [((Mes)PDI(Me))U(THF)]2 (4), were examined using electronic and X-ray absorption spectroscopies, magnetometry, and computational analyses. Taken together, these studies suggest that all members of the series contain uranium(IV) centers with 5f (2) configurations and reduced ligand frameworks, specifically [(Mes)PDI(Me)](•/-), [(Mes)PDI(Me)](2-), [(Mes)PDI(Me)](3-) and [(Mes)PDI(Me)](4-), respectively. In the cases of 2, 3, and 4 no unpaired spin density was found on the ligands, indicating a singlet diradical ligand in monomeric 2 and ligand electron spin-pairing through dimerization in 3 and 4. Interaction energies, representing enthalpies of dimerization, of -116.0 and -144.4 kcal mol(-1) were calculated using DFT for the monomers of 3 and 4, respectively, showing there is a large stabilization gained by dimerization through uranium-arene bonds. Highlighted in these studies is compound 4, bearing a previously unobserved pyridine(diimine) tetraanion, that was uniquely stabilized by backbonding between uranium cations and the η(5)-pyridyl ring.

Mortality (1950–1999) and cancer incidence (1969–1999) of workers in the Port Hope cohort study exposed to a unique combination of radium, uranium and γ-ray doses

PubMed Central

Zablotska, Lydia B; Lane, Rachel S D; Frost, Stanley E

2013-01-01

Objectives Uranium processing workers are exposed to uranium and radium compounds from the ore dust and to γ-ray radiation, but less to radon decay products (RDP), typical of the uranium miners. We examined the risks of these exposures in a cohort of workers from Port Hope radium and uranium refinery and processing plant. Design A retrospective cohort study with carefully documented exposures, which allowed separation of those with primary exposures to radium and uranium. Settings Port Hope, Ontario, Canada, uranium processors with no mining experience. Participants 3000 male and female workers first employed (1932–1980) and followed for mortality (1950–1999) and cancer incidence (1969–1999). Outcome measures Cohort mortality and incidence were compared with the general Canadian population. Poisson regression was used to evaluate the association between cumulative RDP exposures and γ-ray doses and causes of death and cancers potentially related to radium and uranium processing. Results Overall, workers had lower mortality and cancer incidence compared with the general Canadian population. In analyses restricted to men (n=2645), the person-year weighted mean cumulative RDP exposure was 15.9 working level months (WLM) and the mean cumulative whole-body γ-ray dose was 134.4 millisieverts. We observed small, non-statistically significant increases in radiation risks of mortality and incidence of lung cancer due to RDP exposures (excess relative risks/100 WLM=0.21, 95% CI <−0.45 to 1.59 and 0.77, 95% CI <−0.19 to 3.39, respectively), with similar risks for those exposed to radium and uranium. All other causes of death and cancer incidence were not significantly associated with RDP exposures or γ-ray doses or a combination of both. Conclusions In one of the largest cohort studies of workers exposed to radium, uranium and γ-ray doses, no significant radiation-associated risks were observed for any cancer site or cause of death. Continued follow-up and pooling with other cohorts of workers exposed to by-products of radium and uranium processing could provide valuable insight into occupational risks and suspected differences in risk with uranium miners. PMID:23449746

SUMMARY REVIEW OF HEALTH EFFECTS ASSOCIATED WITH HYDROGEN FLUORIDE AND RELATED COMPOUNDS: HEALTH ISSUE ASSESSMENT

EPA Science Inventory

The major natural sources of airborne hydrogen fluoride (HF) are volcanic activity, ocean spray, and crustal weathering of fluoride-containing rocks. Anthropogenic sources include emissions from industrial operations such as aluminum and fluorocarbon production, and uranium proce...

Isolation and structure determination of a new flavone glycoside from seed residues of seabuckthorn (Hippophae rhamnoides L.).

PubMed

Zhou, Wenna; Yuan, Zhenzhen; Li, Gang; Ouyang, Jian; Suo, Yourui; Wang, Honglun

2018-04-01

In this study, a valid method was established for the isolation and purification of flavone glycosides from Hippophae rhamnoides L. seed residues using high-speed counter-current chromatography in one step, with a solvent system of ethyl acetate-methanol-n-butyl alcohol-water (9:1:0.5:9, v/v/v/v). A total of 28.8 mg compound I and 57.3 mg compound II were obtained from 200 mg of flavone H-glycosides rich extract, with purities of 98.3 and 96.4%, respectively. The structures of two compounds were identified by MS and NMR. 3-O-β-D-Sophorosylkaempferol-7-O-{3-O-[2(E)-2,6-dimethyl-6-hydroxyocta-2,7-dienoyl]}-α-L-rhamnoside is compound I and compound II named hippophanone is a new compound were identified by MS and NMR. The method was efficient and convenient, which could be used for the preparative separation of flavone glycosides from H. rhamnoides L. seed residues.

Behavior of Colorado Plateau uranium minerals during oxidation

USGS Publications Warehouse

Garrels, Robert Minard; Christ, C.L.

1956-01-01

Uranium occurs as U(VI) and U(IV) in minerals of the Colorado Plateau ores. The number of species containing U(VI) is large, but only two U(IV) minerals are known from the Plateau: uraninite, and oxide, and coffinite, a hydroxy-silicate. These oxidize to yield U(VI) before reacting significantly with other mineral constituents. Crystal-structure analysis has shown that U(VI) invariable occurs as uranyl ion, UO2+2. Uranyl ion may form complex carbonate or sulfate ions with resulting soluble compounds, but only in the absence of quinquevalent vanadium, arsenic, or phosphorous. In the presence of these elements in the +5 valence state, the uranyl ion is fixed in insoluble layer compounds formed by union of uranyl ion with orthovanadate, orthophosphate, or orthoarsenate. Under favorable conditions UO2+2 may react to form the relatively insoluble rutherfordine, UO2CO3, or hydrated uranyl hydroxides. These are rarely found on the Colorado Plateau as opposed to their excellent development in other uraniferous areas, a condition which is apparently related to the semiarid climate and low water table of the Plateau. Uranium may also be fixed as uranyl silicate, but little is known about minerals of this kind. In the present study emphasis has been placed on a detailing of the chemical and crystal structural changes which occur in the oxidation paragenetic sequence.

Uranium Bio-accumulation and Cycling as revealed by Uranium Isotopes in Naturally Reduced Sediments from the Upper Colorado River Basin

NASA Astrophysics Data System (ADS)

Lefebvre, Pierre; Noël, Vincent; Jemison, Noah; Weaver, Karrie; Bargar, John; Maher, Kate

2016-04-01

Uranium (U) groundwater contamination following oxidized U(VI) releases from weathering of mine tailings is a major concern at numerous sites across the Upper Colorado River Basin (CRB), USA. Uranium(IV)-bearing solids accumulated within naturally reduced zones (NRZs) characterized by elevated organic carbon and iron sulfide compounds. Subsequent re-oxidation of U(IV)solid to U(VI)aqueous then controls the release to groundwater and surface water, resulting in plume persistence and raising public health concerns. Thus, understanding the extent of uranium oxidation and reduction within NRZs is critical for assessing the persistence of the groundwater contamination. In this study, we measured solid-phase uranium isotope fractionation (δ238/235U) of sedimentary core samples from four study sites (Shiprock, NM, Grand Junction, Rifle and Naturita, CO) using a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS). We observe a strong correlation between U accumulation and the extent of isotopic fractionation, with Δ238U up to +1.8 ‰ between uranium-enriched and low concentration zones. The enrichment in the heavy isotopes within the NRZs appears to be especially important in the vadose zone, which is subject to variations in water table depth. According to previous studies, this isotopic signature is consistent with biotic reduction processes associated with metal-reducing bacteria. Positive correlations between the amount of iron sulfides and the accumulation of reduced uranium underline the importance of sulfate-reducing conditions for U(IV) retention. Furthermore, the positive fractionation associated with U reduction observed across all sites despite some variations in magnitude due to site characteristics, shows a regional trend across the Colorado River Basin. The maximum extent of 238U enrichment observed in the NRZ proximal to the water table further suggests that the redox cycling of uranium, with net release of U(VI) to the groundwater by non-fractionating oxidation, is occurring within this zone. Thus, release of uranium from the NRZs may play a critical role in the persistence of groundwater contamination at these sites.

Hydrothermal Synthesis and Crystal Structures of Actinide Compounds

NASA Astrophysics Data System (ADS)

Runde, Wolfgang; Neu, Mary P.

Since the 1950s actinides have been used to benefit industry, science, health, and national security. The largest industrial application, electricity generation from uranium and thorium fuels, is growing worldwide. Thus, more actinides are being mined, produced, used and processed than ever before. The future of nuclear energy hinges on how these increasing amounts of actinides are contained in each stage of the fuel cycle, including disposition. In addition, uranium and plutonium were built up during the Cold War between the United States and the Former Soviet Union for defense purposes and nuclear energy. These stockpiles have been significantly reduced in the last decade.

URANIUM DECONTAMINATION

DOEpatents

Buckingham, J.S.; Carroll, J.L.

1959-12-22

A process is described for reducing the extractability of ruthenium, zirconium, and niobium values into hexone contained in an aqueous nitric acid uranium-containing solution. The solution is made acid-deficient, heated to between 55 and 70 deg C, and at that temperature a water-soluble inorganic thiosulfate is added. By this, a precipitate is formed which carries the bulk of the ruthenium, and the remainder of the ruthenium as well as the zirconium and niobium are converted to a hexone-nonextractable form. The rutheniumcontaining precipitate can either be removed from the solu tion or it can be dissolved as a hexone-non-extractable compound by the addition of sodium dichromate prior to hexone extraction.

Raman spectroscopic investigation of thorium dioxide-uranium dioxide (ThO₂-UO₂) fuel materials.

PubMed

Rao, Rekha; Bhagat, R K; Salke, Nilesh P; Kumar, Arun

2014-01-01

Raman spectroscopic investigations were carried out on proposed nuclear fuel thorium dioxide-uranium dioxide (ThO2-UO2) solid solutions and simulated fuels based on ThO2-UO2. Raman spectra of ThO2-UO2 solid solutions exhibited two-mode behavior in the entire composition range. Variations in mode frequencies and relative intensities of Raman modes enabled estimation of composition, defects, and oxygen stoichiometry in these compounds that are essential for their application. The present study shows that Raman spectroscopy is a simple, promising analytical tool for nondestructive characterization of this important class of nuclear fuel materials.

Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

PubMed

Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

2015-12-01

Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent analytical developments for powder characterization

NASA Astrophysics Data System (ADS)

Brackx, E.; Pages, S.; Dugne, O.; Podor, R.

2015-07-01

Powders and divided solid materials are widely represented as finished or intermediary products in industries as widely varied as foodstuffs, cosmetics, construction, pharmaceuticals, electronic transmission, and energy. Their optimal use requires a mastery of the transformation process based on knowledge of the different phenomena concerned (sintering, chemical reactivity, purity, etc.). Their modelling and understanding need a prior acquisition of sets of data and characteristics which are more or less challenging to obtain. The goal of this study is to present the use of different physico-chemical characterization techniques adapted to uranium-containing powders analyzed either in a raw state or after a specific preparation (ionic polishing). The new developments touched on concern dimensional characterization techniques for grains and pores by image analysis, chemical surface characterization and powder chemical reactivity characterization. The examples discussed are from fabrication process materials used in the nuclear fuel cycle.

Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

PubMed

Bashi, Davoud Salar; Dowom, Samaneh Attaran; Bazzaz, Bibi Sedigheh Fazly; Khanzadeh, Farhad; Soheili, Vahid; Mohammadpour, Ali

2016-05-01

To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L. extracts. Maceration and ultrasound-assisted extraction (UAE) (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1) methanol purity) were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay), MFCs (colony diameter), total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity) was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m.) UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1)) than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1)). Moreover, it (MGI: 2.32-100 %) revealed more anti-mold activity than maceration (MGI: <28.77 %). Explosive disruption of the cell walls, therefore, enhanced extraction yield by acoustic cavitation, was elucidated using SEM. Caffeic acid, tannic acid, quercetin, trans ferulic acid and rosmarinic acid were determined as the phenolic compounds in the optimized extract. RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds.

Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

PubMed Central

Bashi, Davoud Salar; Dowom, Samaneh Attaran; Bazzaz, Bibi Sedigheh Fazly; Khanzadeh, Farhad; Soheili, Vahid; Mohammadpour, Ali

2016-01-01

Objective(s): To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L. extracts. Materials and Methods: Maceration and ultrasound-assisted extraction (UAE) (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1) methanol purity) were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay), MFCs (colony diameter), total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. Results: A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity) was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m.) UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1)) than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1)). Moreover, it (MGI: 2.32-100 %) revealed more anti-mold activity than maceration (MGI: <28.77 %). Explosive disruption of the cell walls, therefore, enhanced extraction yield by acoustic cavitation, was elucidated using SEM. Caffeic acid, tannic acid, quercetin, trans ferulic acid and rosmarinic acid were determined as the phenolic compounds in the optimized extract. Conclusion: RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds. PMID:27403260

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.

Effect of Reaction Period on Stoichiometry, Phase Purity, and Morphology of Hydrothermally Synthesized Cu2NiSnS4 Nanopowder

NASA Astrophysics Data System (ADS)

Babu, G. Sahaya Dennish; Shajan, X. Sahaya; Alwin, S.; Ramasubbu, V.; Balerao, Gopal M.

2018-01-01

The effect of reaction period on the phase purity, morphology, and stoichiometry of Cu2NiSnS4 (CNTS) nanopowder prepared by hydrothermal method has been investigated. Polyvinylpyrrolidone (PVP) and thioglycolic acid were used as capping agent and sulfur source, respectively. The presence of cubic stannite crystal structure and its phase purity were confirmed by powder x-ray diffraction analysis and Raman spectroscopy. Furthermore, the morphological, crystallographic, and optical features of the prepared CNTS nanopowder were characterized by field-emission scanning electron microscopy, transmission electron microscopy, and ultraviolet-visible (UV-Vis) spectrophotometry. The elemental ratios of Cu/(Ni + Sn) and Ni/Sn showed that the stoichiometry of CNTS was maintained for the compounds synthesized at 230°C with reaction period of 24 h. The occurrence of Cu+, Ni2+, Sn4+, and S2- was evaluated by x-ray photoelectron spectroscopy. The prepared material was used as counter electrode in a dye-sensitized solar cell (DSSC) as an alternative to platinum (Pt), resulting in conversion efficiency of 0.92%. These results indicate that CNTS is a prospective material to replace conventional Pt-based counter electrodes in DSSCs.

Hybrid membrane--PSA system for separating oxygen from air

DOEpatents

Staiger, Chad L [Albuquerque, NM; Vaughn, Mark R [Albuquerque, NM; Miller, A Keith [Albuquerque, NM; Cornelius, Christopher J [Blackburg, VA

2011-01-25

A portable, non-cryogenic, oxygen generation system capable of delivering oxygen gas at purities greater than 98% and flow rates of 15 L/min or more is described. The system consists of two major components. The first component is a high efficiency membrane capable of separating argon and a portion of the nitrogen content from air, yielding an oxygen-enriched permeate flow. This is then fed to the second component, a pressure swing adsorption (PSA) unit utilizing a commercially available, but specifically formulated zeolite compound to remove the remainder of the nitrogen from the flow. The system is a unique gas separation system that can operate at ambient temperatures, for producing high purity oxygen for various applications (medical, refining, chemical production, enhanced combustion, fuel cells, etc . . . ) and represents a significant advance compared to current technologies.

Microwave-Facilitated SPOT-Synthesis of Antibacterial Dipeptoids.

PubMed

Schneider, Anne C; Fritz, Daniel; Vasquez, Joseph K; Vollrath, Sidonie B L; Blackwell, Helen E; Bräse, Stefan

2017-12-11

With microwave irradiation, the submonomer synthesis of dipeptoids on functionalized cellulose can be accelerated with good yields and purity. Optimization provided a library of 96 dipeptoids. From these, 29 compounds were found with an antibacterial activity against MRSA at a concentration of 25 μM. Large nonpolar residues, such as undecylamine and dehydroabiethylamine, are the key components engendering the observed antibacterial activity of these peptoids.

JPRS Report, Science & Technology, USSR: Chemistry

DTIC Science & Technology

1990-12-28

Abstract] The study reported herein examined the phase state of jet fuels with different degrees of purity and aging to discover its effect on the...liquid phase oxidation of waste water from various industries was studies . Oxidation was conducted in an autoclave-type apparatus at 200 and 5 Mpa...features of carbonyl compounds. The study reported herein examined the reaction of dialkylalki- nylphosphonites with diethyl ether of mesoxalic acid

Uranium Sequestration During Biostimulated Reduction and In Response to the Return of Oxic Conditions In Shallow Aquifers

USGS Publications Warehouse

Fuller, Christopher C.; Johnson, Kelly J.; Akstin, Katherine; Singer, David M.; Yabusaki, Steven B.; Fang, Yilin; Fuhrmann, M.

2015-01-01

A proposed approach for groundwater remediation of uranium contamination is to generate reducing conditions by stimulating the growth of microbial populations through injection of electron donor compounds into the subsurface. Sufficiently reducing conditions will result in reduction of soluble hexavalent uranium, U(VI), and precipitation of the less soluble +4 oxidation state uranium, U(IV). This process is termed biostimulated reduction. A key issue in the remediation of uranium (U) contamination in aquifers by biostimulated reduction is the long term stability of the sequestered uranium. Three flow-through column experiments using aquifer sediment were used to evaluate the remobilization of bioreduced U sequestered under conditions in which biostimulation extended well into sulfate reduction to enhance precipitation of reduced sulfur phases such as iron sulfides. One column received added ferrous iron, Fe(II), increasing production of iron sulfides, to test their effect on remobilization of the sequestered uranium, either by serving as a redox buffer by competing for dissolved oxygen, or by armoring the reduced uranium. During biostimulation of the ambient microbial population with acetate, dissolved uranium was lowered by a factor of 2.5 or more with continued removal for over 110 days of biostimulation, well after the onset of sulfate reduction at ~30 days. Sequestered uranium was essentially all U(IV) resulting from the formation of nano-particulate uraninite that coated sediment grains to a thickness of a few 10’s of microns, sometimes in association with S and Fe. A multicomponent biogeochemical reactive transport model simulation of column effluents during biostimulation was generally able to describe the acetate oxidation, iron, sulfate, and uranium reduction for all three columns using parameters derived from simulations of field scale biostimulation experiments. Columns were eluted with artificial groundwater at equilibrium with atmospheric oxygen to simulate the upper limit of dissolved oxygen in recharge water. Overall about 9% of total uranium removed from solution during biostimulation was remobilized. Release of U during oxic elution was a continuous process over 140 days with dissolved uranium concentrations about 0.2 and 0.8 aM for columns with and without ferrous iron addition, respectively. Uranium remaining on the sediment was in the reduced form. The prolonged period of biostimulation and concomitant sulfate reduction appears to limit the rate of U(IV) oxidative remobilization in contrast to a large release observed for columns in previous studies that did not undergo sulfate reduction. Although continued sulfate reduction may cause decreased permeability from precipitation of iron sulfide, the greater apparent stability of the sequestered U(IV) provided by the sustained biostimulation should be considered in design of field scale remediation efforts. Remobilization of uranium following biostimulated reduction should be tested further at the field scale.

Solubility testing of actinides on breathing-zone and area air samples

NASA Astrophysics Data System (ADS)

Metzger, Robert Lawrence

The solubility of inhaled radionuclides in the human lung is an important characteristic of the compounds needed to perform internal dosimetry assessments for exposed workers. A solubility testing method for uranium and several common actinides has been developed with sufficient sensitivity to allow profiles to be determined from routine breathing zone and area air samples in the workplace. Air samples are covered with a clean filter to form a filter-sample-filter sandwich which is immersed in an extracellular lung serum simulant solution. The sample is moved to a fresh beaker of the lung fluid simulant each day for one week, and then weekly until the end of the 28 day test period. The soak solutions are wet ashed with nitric acid and hydrogen peroxide to destroy the organic components of the lung simulant solution prior to extraction of the nuclides of interest directly into an extractive scintillator for subsequent counting on a Photon-Electron Rejecting Alpha Liquid Scintillation (PERALSsp°ler ) spectrometer. Solvent extraction methods utilizing the extractive scintillators have been developed for the isotopes of uranium, plutonium, and curium. The procedures normally produce an isotopic recovery greater than 95% and have been used to develop solubility profiles from air samples with 40 pCi or less of Usb3Osb8. This makes it possible to characterize solubility profiles in every section of operating facilities where airborne nuclides are found using common breathing zone air samples. The new method was evaluated by analyzing uranium compounds from two uranium mills whose product had been previously analyzed by in vitro solubility testing in the laboratory and in vivo solubility testing in rodents. The new technique compared well with the in vivo rodent solubility profiles. The method was then used to evaluate the solubility profiles in all process sections of an operating in situ uranium plant using breathing zone and area air samples collected during routine plant operations. The solubility profiles developed from this work showed excellent agreement with the results of the worker urine bioassay program at the plant and identified a significant error in existing internal dose assessments at this facility.

Chelation of UO(2)(2+) by vitamin B6 complex derivatives: synthesis and characterization of [UO2(beta-pyracinide)2(H2O)] and [UO2(Pyr2en)DMSO]Cl2{Pyr2en=N,N'-ethylenebis(pyridoxylideneiminato)}. A useful modeling of assimilation of uranium by living beings.

PubMed

Back, Davi Fernando; de Oliveira, Gelson Manzoni; Lang, Ernesto Schulz

2006-10-01

The vitamin B(6) derivatives 4-pyridoxic acid (anionic) and the Schiff base N,N'-ethylenebis(pyridoxylideneiminato) react with UO(2)(NO(3))(2) * 6H(2)O to give [UO(2)(beta-pyracinide)(2)(H(2)O)] (beta-pyracin=4-pyridoxic acid) and [UO(2)(Pyr(2)en)DMSO]Cl(2)(Pyr(2)en=N,N'-ethylenebis(pyridoxylideneiminato); DMSO=dimethyl sulfoxide). In both compounds the two uranyl oxo ligands set the axis of distorted pentagonal bipyramides. The ability of vitamin B(6) derivatives to react with UO(2)(2+) allowing the chelation of one uranium atom represents a very specific model of assimilation of uranium by living beings. It could also explain the serious damages caused by heavy or radioactive metals like uranium since their complexation "in vivo" by enzymatic systems like pyridoxal phosphate-containing enzymes would lead to a modification of the prosthetic groups of the metalloenzymes with loss of their catalytic activities.

Critical Amounts of Uranium Compounds

DOE R&D Accomplishments Database

Konopinski, E.; Metropolis, N.; Teller, E.; Woods, L.

1943-03-19

The method of calculation of critical masses of oxides and fluorides of U is given. The geometry assumed is a sphere and the calculations hold only in the absence of hydrogenous materials. Calculations are carried out which are applicable to materials containing form 20 to 100% U{sup 235}. (T.R.H.)

Synthesis and synergistic, additive inhibitory effects of novel spiro derivatives against ringworm infections.

PubMed

Sharma, Gajanand; Sharma, Richa; Dandia, Anshu; Bansal, Preeti

2013-01-01

An environmentally benign solvent free synthesis of various spiro-1,4-dihydropyridines (1,4-DHPs) incorporating 2-oxindole/piperidines is performed in 5-8 min with reasonable purity in 80-90% yield under microwave irradiation using montmorillonite KSF as an inorganic solid support. The reaction is found to be general with respect to various cyclic carbonyl compounds, e.g. cyclohexanone, substituted indole-2,3-dione, and piperidinone derivatives. In our study, these compounds were also found effective against dermatophytes and other fungal organisms. Our results suggest that novel spiro derivatives can be used for the treatment of dermatophytosis or ringworm infections.

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.

Highly Sensitive Detection of UV Radiation Using a Uranium Coordination Polymer.

PubMed

Liu, Wei; Dai, Xing; Xie, Jian; Silver, Mark A; Zhang, Duo; Wang, Yanlong; Cai, Yawen; Diwu, Juan; Wang, Jian; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao

2018-02-07

The accurate detection of UV radiation is required in a wide range of chemical industries and environmental or biological related applications. Conventional methods taking advantage of semiconductor photodetectors suffer from several drawbacks such as sophisticated synthesis and manufacturing procedure, not being able to measure the accumulated UV dosage as well as high defect density in the material. Searching for new strategies or materials serving as precise UV dosage sensor with extremely low detection limit is still highly desirable. In this work, a radiation resistant uranium coordination polymer [UO 2 (L)(DMF)] (L = 5-nitroisophthalic acid, DMF = N,N-dimethylformamide, denoted as compound 1) was successfully synthesized through mild solvothermal method and investigated as a unique UV probe with the detection limit of 2.4 × 10 -7 J. On the basis of the UV dosage dependent luminescence spectra, EPR analysis, single crystal structure investigation, and the DFT calculation, the UV-induced radical quenching mechanism was confirmed. Importantly, the generated radicals are of significant stability which offers the opportunity for measuring the accumulated UV radiation dosage. Furthermore, the powder material of compound 1 was further upgraded into membrane material without loss in luminescence intensity to investigate the real application potentials. To the best of our knowledge, compound 1 represents the most sensitive coordination polymer based UV dosage probe reported to date.

Adamantoylated biologically active small peptides and glycopeptides structurally related to the bacterial peptidoglycan.

PubMed

Frkanec, Ruža; Vranešić, Branka; Tomić, Srdjanka

2013-01-01

A large number of novel synthetic compounds representing smaller parts of original peptidoglycan molecules have been synthesized and found to possess versatile biological activity, particularly immunomodulating properties. A series of compounds containing the adamantyl residues coupled to peptides and glycopeptides characteristic for bacterial peptidoglycan was described. The new adamantylpeptides and adamantylglycopeptides were prepared starting from N-protected racemic adamantylglycine and dipeptide L-Ala-D-isoglutamine. The adamantyl glycopeptides were obtained by coupling the adamantyltripeptides with alpha-D-mannose moiety through spacer molecule of fixed chirality. Since the starting material was D,L-(adamantyl-glycine) the condensation products with the dipeptide were mixtures of diastereoisomers. The obtained diastereoisomers were separated, characterized, and tested for immunostimulating activity. An HPLC method for purity testing was developed and adapted for the particular compounds.

Measurement and simulation of a Compton suppression system for safeguards application

NASA Astrophysics Data System (ADS)

Lee, Seung Kyu; Seo, Hee; Won, Byung-Hee; Lee, Chaehun; Shin, Hee-Sung; Na, Sang-Ho; Song, Dae-Yong; Kim, Ho-Dong; Park, Geun-Il; Park, Se-Hwan

2015-11-01

Plutonium (Pu) contents in spent nuclear fuels, recovered uranium (U) or uranium/transuranium (U/TRU) products must be measured in order to secure the safeguardability of a pyroprocessing facility. Self-induced X-Ray fluorescence (XRF) and gamma-ray spectroscopy are useful techniques for determining Pu-to-U ratios and Pu isotope ratios of spent fuel. Photon measurements of spent nuclear fuel by using high-resolution spectrometers such as high-purity germanium (HPGe) detectors show a large continuum background in the low-energy region, which is due in large part to Compton scattering of energetic gamma rays. This paper proposes a Compton suppression system for reducing of the Compton continuum background. In the present study, the system was configured by using an HPGe main detector and a BGO (bismuth germanate: Bi4Ge3O12) guard detector. The system performances for gamma-ray measurement and XRF were evaluated by means of Monte Carlo simulations and measurements of the radiation source. The Monte Carlo N-Particle eXtended (MCNPX) simulations were performed using the same geometry as for the experiments, and considered, for exact results, the production of secondary electrons and photons. As a performance test of the Compton suppression system, the peak-to-Compton ratio, which is a figure of merit to evaluate the gamma-ray detection, was enhanced by a factor of three or more when the Compton suppression system was used.

Summary of ORSphere Critical and Reactor Physics Measurements

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

Marshall, Margaret A.; Bess, John D.

In the early 1970s Dr. John T. Mihalczo (team leader), J. J. Lynn, and J. R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950s. The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared with the GODIVAmore » I experiments. This critical configuration has been evaluated. Preliminary results were presented at ND2013. Since then, the evaluation was finalized and judged to be an acceptable benchmark experiment for the International Criticality Safety Benchmark Experiment Project (ICSBEP). Additionally, reactor physics measurements were performed to determine surface button worths, central void worth, delayed neutron fraction, prompt neutron decay constant, fission density and neutron importance. These measurements have been evaluated and found to be acceptable experiments and are discussed in full detail in the International Handbook of Evaluated Reactor Physics Benchmark Experiments. The purpose of this paper is summary summarize all the critical and reactor physics measurements evaluations and, when possible, to compare them to GODIVA experiment results.« less

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

Margaret A. Marshall

In the early 1970’s Dr. John T. Mihalczo (team leader), J.J. Lynn, and J.R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) in an attempt to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950’s (HEU-MET-FAST-001). The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared withmore » the GODIVA I experiments. “The very accurate description of this sphere, as assembled, establishes it as an ideal benchmark for calculational methods and cross-section data files.” (Reference 1) While performing the ORSphere experiments care was taken to accurately document component dimensions (±0. 0001 in. for non-spherical parts), masses (±0.01 g), and material data The experiment was also set up to minimize the amount of structural material in the sphere proximity. A three part sphere was initially assembled with an average radius of 3.4665 in. and was then machined down to an average radius of 3.4420 in. (3.4425 in. nominal). These two spherical configurations were evaluated and judged to be acceptable benchmark experiments; however, the two experiments are highly correlated.« less

Are We There Yet? Applying Thermodynamic and Kinetic Profiling on Embryonic Ectoderm Development (EED) Hit-to-Lead Program.

PubMed

Wang, Ying; Edalji, Rohinton P; Panchal, Sanjay C; Sun, Chaohong; Djuric, Stevan W; Vasudevan, Anil

2017-10-26

It is advocated that kinetic and thermodynamic profiling of bioactive compounds should be incorporated and utilized as complementary tools for hit and lead optimizations in drug discovery. To assess their applications in the EED hit-to-lead optimization process, large amount of thermodynamic and kinetic data were collected and analyzed via isothermal titration calorimetry (ITC) and surface plasmon resonance (SPR), respectively. Slower dissociation rates (k off ) of the lead compounds were observed as the program progressed. Analysis of the kinetic data indicated that compound cellular activity correlated with both K i and k off . Our analysis revealed that ITC data should be interpreted in the context of chiral purity of the compounds. The thermodynamic signatures of the EED aminopyrrolidine compounds were found to be mainly enthalpy driven with improved enthalpic contributions as the program progressed. Our study also demonstrated that significant challenges still exist in utilizing kinetic and thermodynamic parameters for hit selection.

Mitigation of Hydrogen Gas Generation from the Reaction of Uranium Metal with Water in K Basin Sludge and Sludge Waste Forms

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

Sinkov, Sergey I.; Delegard, Calvin H.; Schmidt, Andrew J.

2011-06-08

Prior laboratory testing identified sodium nitrate and nitrite to be the most promising agents to minimize hydrogen generation from uranium metal aqueous corrosion in Hanford Site K Basin sludge. Of the two, nitrate was determined to be better because of higher chemical capacity, lower toxicity, more reliable efficacy, and fewer side reactions than nitrite. The present lab tests were run to determine if nitrate’s beneficial effects to lower H2 generation in simulated and genuine sludge continued for simulated sludge mixed with agents to immobilize water to help meet the Waste Isolation Pilot Plant (WIPP) waste acceptance drainable liquid criterion. Testsmore » were run at ~60°C, 80°C, and 95°C using near spherical high-purity uranium metal beads and simulated sludge to emulate uranium-rich KW containerized sludge currently residing in engineered containers KW-210 and KW-220. Immobilization agents tested were Portland cement (PC), a commercial blend of PC with sepiolite clay (Aquaset II H), granulated sepiolite clay (Aquaset II G), and sepiolite clay powder (Aquaset II). In all cases except tests with Aquaset II G, the simulated sludge was mixed intimately with the immobilization agent before testing commenced. For the granulated Aquaset II G clay was added to the top of the settled sludge/solution mixture according to manufacturer application directions. The gas volumes and compositions, uranium metal corrosion mass losses, and nitrite, ammonia, and hydroxide concentrations in the interstitial solutions were measured. Uranium metal corrosion rates were compared with rates forecast from the known uranium metal anoxic water corrosion rate law. The ratios of the forecast to the observed rates were calculated to find the corrosion rate attenuation factors. Hydrogen quantities also were measured and compared with quantities expected based on non-attenuated H2 generation at the full forecast anoxic corrosion rate to arrive at H2 attenuation factors. The uranium metal corrosion rates in water alone and in simulated sludge were near or slightly below the metal-in-water rate while nitrate-free sludge/Aquaset II decreased rates by about a factor of 3. Addition of 1 M nitrate to simulated sludge decreased the corrosion rate by a factor of ~5 while 1 M nitrate in sludge/Aquaset II mixtures decreased the corrosion rate by ~2.5 compared with the nitrate-free analogues. Mixtures of simulated sludge with Aquaset II treated with 1 M nitrate had uranium corrosion rates about a factor of 8 to 10 lower than the water-only rate law. Nitrate was found to provide substantial hydrogen mitigation for immobilized simulant sludge waste forms containing Aquaset II or Aquaset II G clay. Hydrogen attenuation factors of 1000 or greater were determined at 60°C for sludge-clay mixtures at 1 M nitrate. Hydrogen mitigation for tests with PC and Aquaset II H (which contains PC) were inconclusive because of suspected failure to overcome induction times and fully enter into anoxic corrosion. Lessening of hydrogen attenuation at ~80°C and ~95°C for simulated sludge and Aquaset II was observed with attenuation factors around 100 to 200 at 1 M nitrate. Valuable additional information has been obtained on the ability of nitrate to attenuate hydrogen gas generation from solution, simulant K Basin sludge, and simulant sludge with immobilization agents. Details on characteristics of the associated reactions were also obtained. The present testing confirms prior work which indicates that nitrate is an effective agent to attenuate hydrogen from uranium metal corrosion in water and simulated K Basin sludge to show that it is also effective in potential candidate solidified K Basin waste forms for WIPP disposal. The hydrogen mitigation afforded by nitrate appears to be sufficient to meet the hydrogen generation limits for shipping various sludge waste streams based on uranium metal concentrations and assumed waste form loadings.« less

Geology of uranium in the Chadron area, Nebraska and South Dakota

USGS Publications Warehouse

Dunham, Robert Jacob

1961-01-01

The Chadron area covers 375 square miles about 25 miles southeast of the Black Hills. Recurrent mild tectonic activity and erosion on the Chadron arch, a compound anticlinal uplift of regional extent, exposed 1900 feet of Upper Cretaceous rocks, mostly marine shale containing pyrite and organic matter, and 600 feet of Oligocene and Miocene rocks, mostly terrestrial fine-grained sediment containing volcanic ash. Each Cretaceous formation truncated by the sub-Oligocene unconformity is stained yellow and red, leached, kaolinized, and otherwise altered to depths as great as 55 feet. The composition and profile of the altered material indicate lateritic soil; indirect evidence indicates Eocene(?) age. In a belt through the central part of the area, the Brule formation of Oligocene age is a sequence of bedded gypsum, clay, dolomite, and limestone more than 300 feet thick. Uranium in Cretaceous shale in 58 samples averages 0.002 percent, ten times the average for the earths crust. Association with pyrite and organic matter indicates low valency. The uranium probably is syngenetic or nearly so. Uranium in Eocene(?) soil in 43 samples averages 0.054 percent, ranging up to 1.12 percent. The upper part of the soil is depleted in uranium; enriched masses in the basal part of the soil consist of remnants of bedrock shale and are restricted to the highest reaches of the ancient oxidation-reduction interface. The uranium is probably in the from of a low-valent mineral, perhaps uraninite. Modern weathering of Cretaceous shale is capable of releasing as much as 0.780 ppm uranium to water. Eocene(?) weathering probably caused enrichment of the ancient soil through 1) leaching of Cretaceous shale, 2) downward migration of uranyl complex ions, and 3) reduction of hydrogen sulfide at the water table. Uranium minerals occur in the basal 25 feet of the gypsum facies of the Brule formation at the two localities where the gypsum is carbonaceous; 16 samples average 0.066 percent uranium and range up to 0.43 percent. Elsewhere uranium in dolomite and limestone in the basal 25 feet of the gypsum facies in 10 samples averages 0.007 percent, ranging up to 0.12 percent. Localization of the uranium at the base of the gypsum facies suggests downward moving waters; indirect evidence that the water from which the gypsum was deposited was highly alkaline suggests that the uranium was leached from volcanic ash in Oligocene time.

Hybrid composites : combining cellulose fibers and wollastonite mineral fibers into a nylon 6 matrix

Treesearch

Rodney E. Jacobson; Daniel F. Caulfield

2003-01-01

The objective of this research was to develop a high purity cellulose/wollastonite pellet that could then be accurately metered and feed into a laboratory scale twin-screw extruder and compounded with a nylon 6 resin. The major focus was targeted on a 20 percent cellulose/20 percent wollastonite/60 percent nylon 6 composite. Limited research with nylon 6,6 resins was...

Development and validation of an LC-UV method for the quantification and purity determination of the novel anticancer agent C1311 and its pharmaceutical dosage form.

PubMed

den Brok, Monique W J; Nuijen, Bastiaan; Hillebrand, Michel J X; Grieshaber, Charles K; Harvey, Michael D; Beijnen, Jos H

2005-09-01

C1311 (5-[[2-(diethylamino)ethyl]amino]-8-hydroxyimidazo [4,5,1-de]-acridin-6-one-dihydrochloride trihydrate) is the lead compound from the group of imidazoacridinones, a novel group of rationally designed anticancer agents. The pharmaceutical development of C1311 necessitated the availability of an assay for the quantification and purity determination of C1311 active pharmaceutical ingredient (API) and its pharmaceutical dosage form. A reversed-phase liquid chromatographic method (RP-LC) with ultraviolet (UV) detection was developed, consisting of separation on a C18 column with phosphate buffer (60 mM; pH 3 with 1 M citric acid)-acetonitrile-triethylamine (83:17:0.05, v/v/v) as the mobile phase and UV-detection at 280 nm. The method was found to be linear over a concentration range of 2.50-100 microg/mL, precise and accurate. Accelerated stress testing showed degradation products, which were well separated from the parent compound, confirming its stability-indicating capacity. Moreover, the use of LC-MS and on-line photo diode array detection enabled us to propose structures for four degradation products. Two of these products were also found as impurities in the API and more abundantly in an impure lot of API.

In situ ligand synthesis with the UO22+ cation under hydrothermal conditions

NASA Astrophysics Data System (ADS)

Frisch, Mark; Cahill, Christopher L.

2007-09-01

A novel uranium (VI) coordination polymer, (UO 2) 2(C 2O 4)(C 5H 6NO 3) 2 ( 1), has been prepared under the hydrothermal reaction of uranium nitrate hexahydrate and L-pyroglutamic acid. Compound 1 (monoclinic, C2/ c, a=22.541(6) Å, b=5.7428(15) Å, c=15.815(4) Å, β=119.112(4)°, Z=4, R1=0.0237, w R2=0.0367) consists of uranium pentagonal bipyramids linked via L-pyroglutamate and oxalate anions to form an overall two-dimensional (2D) structure. With the absence of oxalic acid within the starting materials, the oxalate anions are hypothesized to form in situ whereby decarboxylation of L-pyroglutamic acid occurs followed by coupling of CO 2 to form the oxalate linkages as observed in the crystal structure. Addition of copper (II) to this system appears to promote oxalate formation in that synthetic moolooite (Cu(C 2O 4)· nH 2O; 0⩽ n⩽1) and a known uranyl oxalate [(UO 2) 2(C 2O 4)(OH) 2(H 2O) 2·H 2O], co-crystallize in significant quantity. Compound 1 exhibits the characteristic uranyl emission spectrum upon either direct uranyl excitation or ligand excitation, the latter of which shows an increase in relative intensity. This subsequent increase in the intensity indicates an energy transfer from the ligand to the uranyl cations thus illustrating an example of the antenna effect in the solid state.

Facile CO Cleavage by a Multimetallic CsU2 Nitride Complex.

PubMed

Falcone, Marta; Kefalidis, Christos E; Scopelliti, Rosario; Maron, Laurent; Mazzanti, Marinella

2016-09-26

Uranium nitrides are important materials with potential for application as fuels for nuclear power generation, and as highly active catalysts. Molecular nitride compounds could provide important insight into the nature of the uranium-nitride bond, but currently little is known about their reactivity. In this study, we found that a complex containing a nitride bridging two uranium centers and a cesium cation readily cleaved the C≡O bond (one of the strongest bonds in nature) under ambient conditions. The product formed has a [CsU2 (μ-CN)(μ-O)] core, thus indicating that the three cations cooperate to cleave CO. Moreover, the addition of MeOTf to the nitride complex led to an exceptional valence disproportionation of the CsU(IV) -N-U(IV) core to yield CsU(III) (OTf) and [MeN=U(V) ] fragments. The important role of multimetallic cooperativity in both reactions is illustrated by the computed reaction mechanisms. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Efficient hit-finding approaches for histone methyltransferases: the key parameters.

PubMed

Ahrens, Thomas; Bergner, Andreas; Sheppard, David; Hafenbradl, Doris

2012-01-01

For many novel epigenetics targets the chemical ligand space and structural information were limited until recently and are still largely unknown for some targets. Hit-finding campaigns are therefore dependent on large and chemically diverse libraries. In the specific case of the histone methyltransferase G9a, the authors have been able to apply an efficient process of intelligent selection of compounds for primary screening, rather than screening the full diverse deck of 900 000 compounds to identify hit compounds. A number of different virtual screening methods have been applied for the compound selection, and the results have been analyzed in the context of their individual success rates. For the primary screening of 2112 compounds, a FlashPlate assay format and full-length histone H3.1 substrate were employed. Validation of hit compounds was performed using the orthogonal fluorescence lifetime technology. Rated by purity and IC(50) value, 18 compounds (0.9% of compound screening deck) were finally considered validated primary G9a hits. The hit-finding approach has led to novel chemotypes being identified, which can facilitate hit-to-lead projects. This study demonstrates the power of virtual screening technologies for novel, therapeutically relevant epigenetics protein targets.

Synthesis and in vivo anticonvulsant activity of 2-methyl-2-[3-(5-piperazin-1-yl-[1,3,4]oxadiazol-2-yl)-phenyl]-propionitrile derivatives.

PubMed

Harish, Kikkeri P; Mohana, Kikkeri N; Mallesha, Lingappa; Veeresh, Bantal

2014-04-01

A series of new 2-methyl-2-[3-(5-piperazin-1-yl-[1,3,4]oxadiazol-2-yl)-phenyl]-propionitrile derivatives 8a-o, 9a-c, 10a-d, and 11a-d were synthesized to meet the structural requirements essential for anticonvulsant property. The structures of all the synthesized compounds were confirmed by means of (1)H NMR, (13)C NMR, and mass spectral studies. The purity of the novel compounds was confirmed by elemental analyses. All the compounds were screened for their anticonvulsant activity against maximal electroshock (MES) seizure method and their neurotoxic effects were determined by rotorod test. Compounds 8d, 8e, and 8f were found to be the most potent of this series. The same compounds showed no neurotoxicity at the maximum dose administered (100 mg/kg). The efforts were also made to establish the structure-activity relationships among the synthesized compounds. The pharmacophore model was used to validate the anticonvulsant activity of the synthesized molecules. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Induction of cellular and molecular immunomodulatory pathways by vitamin A and Flavonoids

PubMed Central

Patel, Sapna; Vajdy, Michael

2016-01-01

Introduction A detailed study of reports on the immunomodulatory properties of vitamin A and select flavonoids may pave the way for using these natural compounds or compounds with similar structures in novel drug and vaccine designs against infectious and autoimmune diseases and cancers. Areas Covered Intracellular transduction pathways, cellular differentiation and functional immunomodulatory responses have been reviewed. The reported studies encompass in vitro, in vivo preclinical and clinical studies that address the role of Vitamin A and select flavonoids in induction of innate and adaptive B and T cell responses, including TH1, TH2 and Treg. Expert Opinion While the immunomodulatory role of vitamin A, and related compounds, is well-established in many preclinical studies, its role in humans has begun to gain wider acceptance. In contrast, the role of flavonoids is mostly controversial in clinical trials, due to the diversity of the various classes of these compounds, and possibly due to the purity and the selected doses of the compounds. However, current preclinical and clinical studies warrant further detailed studies of these promising immuno-modulatory compounds. PMID:26185959

Nano-scaled top-down of bismuth chalcogenides based on electrochemical lithium intercalation

NASA Astrophysics Data System (ADS)

Chen, Jikun; Zhu, Yingjie; Chen, Nuofu; Liu, Xinling; Sun, Zhengliang; Huang, Zhenghong; Kang, Feiyu; Gao, Qiuming; Jiang, Jun; Chen, Lidong

2011-12-01

A two-step method has been used to fabricate nano-particles of layer-structured bismuth chalcogenide compounds, including Bi2Te3, Bi2Se3, and Bi2Se0.3Te2.7, through a nano-scaled top-down route. In the first step, lithium (Li) atoms are intercalated between the van der Waals bonded quintuple layers of bismuth chalcogenide compounds by controllable electrochemical process inside self-designed lithium ion batteries. And in the second step, the Li intercalated bismuth chalcogenides are subsequently exposed to ethanol, in which process the intercalated Li atoms would explode like atom-scaled bombs to exfoliate original microscaled powder into nano-scaled particles with size around 10 nm. The influence of lithium intercalation speed and amount to three types of bismuth chalcogenide compounds are compared and the optimized intercalation conditions are explored. As to maintain the phase purity of the final nano-particle product, the intercalation lithium amount should be well controlled in Se contained bismuth chalcogenide compounds. Besides, compared with binary bismuth chalcogenide compound, lower lithium intercalation speed should be applied in ternary bismuth chalcogenide compound.

Limits on uranium and thorium bulk content in GERDA Phase I detectors

NASA Astrophysics Data System (ADS)

Collaboration, Gerda; Agostini, M.; Allardt, M.; Bakalyarov, A. M.; Balata, M.; Barabanov, I.; Baudis, L.; Bauer, C.; Becerici-Schmidt, N.; Bellotti, E.; Belogurov, S.; Belyaev, S. T.; Benato, G.; Bettini, A.; Bezrukov, L.; Bode, T.; Borowicz, D.; Brudanin, V.; Brugnera, R.; Caldwell, A.; Cattadori, C.; Chernogorov, A.; D'Andrea, V.; Demidova, E. V.; di Vacri, A.; Domula, A.; Doroshkevich, E.; Egorov, V.; Falkenstein, R.; Fedorova, O.; Freund, K.; Frodyma, N.; Gangapshev, A.; Garfagnini, A.; Grabmayr, P.; Gurentsov, V.; Gusev, K.; Hakemüller, J.; Hegai, A.; Heisel, M.; Hemmer, S.; Hofmann, W.; Hult, M.; Inzhechik, L. V.; Janicskó Csáthy, J.; Jochum, J.; Junker, M.; Kazalov, V.; Kihm, T.; Kirpichnikov, I. V.; Kirsch, A.; Kish, A.; Klimenko, A.; Kneißl, R.; Knöpfle, K. T.; Kochetov, O.; Kornoukhov, V. N.; Kuzminov, V. V.; Laubenstein, M.; Lazzaro, A.; Lebedev, V. I.; Lehnert, B.; Liao, H. Y.; Lindner, M.; Lippi, I.; Lubashevskiy, A.; Lubsandorzhiev, B.; Lutter, G.; Macolino, C.; Majorovits, B.; Maneschg, W.; Medinaceli, E.; Mingazheva, R.; Misiaszek, M.; Moseev, P.; Nemchenok, I.; Palioselitis, D.; Panas, K.; Pandola, L.; Pelczar, K.; Pullia, A.; Riboldi, S.; Rumyantseva, N.; Sada, C.; Salamida, F.; Salathe, M.; Schmitt, C.; Schneider, B.; Schönert, S.; Schreiner, J.; Schütz, A.-K.; Schulz, O.; Schwingenheuer, B.; Selivanenko, O.; Shevchik, E.; Shirchenko, M.; Simgen, H.; Smolnikov, A.; Stanco, L.; Stepaniuk, M.; Vanhoefer, L.; Vasenko, A. A.; Veresnikova, A.; von Sturm, K.; Wagner, V.; Walter, M.; Wegmann, A.; Wester, T.; Wiesinger, C.; Wojcik, M.; Yanovich, E.; Zhitnikov, I.; Zhukov, S. V.; Zinatulina, D.; Zuber, K.; Zuzel, G.

2017-05-01

Internal contaminations of 238U, 235U and 232Th in the bulk of high purity germanium detectors are potential backgrounds for experiments searching for neutrinoless double beta decay of 76Ge. The data from GERDA Phase I have been analyzed for alpha events from the decay chain of these contaminations by looking for full decay chains and for time correlations between successive decays in the same detector. No candidate events for a full chain have been found. Upper limits on the activities in the range of a few nBq/kg for 226Ra, 227Ac and 228Th, the long-lived daughter nuclides of 238U, 235U and 232Th, respectively, have been derived. With these upper limits a background index in the energy region of interest from 226Ra and 228Th contamination is estimated which satisfies the prerequisites of a future ton scale germanium double beta decay experiment.

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

Large-scale purification of 90Sr from nuclear waste materials for production of 90Y, a therapeutic medical radioisotope.

PubMed

Wester, Dennis W; Steele, Richard T; Rinehart, Donald E; DesChane, Jaquetta R; Carson, Katharine J; Rapko, Brian M; Tenforde, Thomas S

2003-07-01

A major limitation on the supply of the short-lived medical isotope 90Y (t1/2 = 64 h) is the available quantity of highly purified 90Sr generator material. A radiochemical production campaign was therefore undertaken to purify 1,500 Ci of 90Sr that had been isolated from fission waste materials. A series of alkaline precipitation steps removed all detectable traces of 137Cs, alpha emitters, and uranium and transuranic elements. Technical obstacles such as the buildup of gas pressure generated upon mixing large quantities of acid with solid 90Sr carbonate were overcome through safety features incorporated into the custom-built equipment used for 90Sr purification. Methods are described for analyzing the chemical and radiochemical purity of the final product and for accurately determining by gravimetry the quantities of 90Sr immobilized on stainless steel filters for future use.

Application of PIXE to the study of Renaissance style enamelled gold jewelry

NASA Astrophysics Data System (ADS)

Weldon, M.; Carlson, J.; Reedy, S.; Swann, C. P.

1996-04-01

This study examines and compares three pieces of Renaissance style gold and enamelled jewelry owned by the Walters Art Gallery, Baltimore, MD, USA. These are a 16th century Hat Badge of Adam and Eve, a 19th century Fortitude Pendant and a Diana Pendant presumed to be of the 16th century (The Walters Art Gallery, Jewelry, Ancient to Modern (Viking, New York, 1979)), Ref. [1]. PIXE spectroscopy was applied to examine the elemental composition of the gold and of the enamels. Compositional differences, including the use of post-Renaissance colorants, were found between the enamels in separate regions of each of the three pieces. The modern colorant, chromium, was, in fact, found in all of the pieces and uranium was found in only the Diana Pendant. There are some differences in the gold purity of the three objects; there are significant differences in the solders used even within one object, the Fortitude Pendant.

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.

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.

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.

Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

PubMed

Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

2017-06-01

The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparative isolation and purification of indigo and indirubin from Folium isatidis by high-speed counter-current chromatography.

PubMed

Lü, Hai-tao; Liu, Jing; Deng, Rui; Song, Ji-ying

2012-01-01

Indigo and indirubin are the main active ingredients found in traditional Chinese herbal medicine Folium isatidis. An effective method for the isolation and purification of indigo and indirubin from Folium isatidis is needed. Compared with the conventional column chromatographic techniques, high-speed counter-current chromatography (HSCCC) is a suitable alternative for the enrichment and purification of these target compounds, and eliminates the complications resulting from a solid support matrix. To develop a reliable HSCCC method for isolation and identification of indigo and indirubin in a one-step separation from Folium isatidis. The optimum extracting conditions of indigo and indirubin from Folium isatidis were investigated by orthogonal test L(16) (4(5)). The target compounds were isolated and purified with a solvent system of n-hexane:ethyl acetate:ethanol:water (1:1:1:1, v/v) and the lower phase was used as the mobile phase in the head-to-tail elution mode. The purities of target compounds were tested by HPLC and their structures were identified by UV, IR, electrospray ion source (ESI)-MS, (1) H-NMR and (13) C-NMR analyses. From 165 mg of the crude extract, 5.65 mg of indigo and 1.00 mg of indirubin were obtained by HPLC analysis with purities of 98.4% and 99.0% respectively, and their mean recoveries were 91.0% and 90.7%, respectively. The HSCCC method is effective for the preparative separation and purification of indigo and indirubin in a one-step separation from Folium isatidis. Copyright © 2012 John Wiley & Sons, Ltd.

Characterisation of Pomegranate-Husk Polyphenols and Semi-Preparative Fractionation of Punicalagin.

PubMed

Aguilar-Zárate, Pedro; Wong-Paz, Jorge E; Michel, Mariela; Buenrostro-Figueroa, Juan; Díaz, Hugo R; Ascacio, Juan A; Contreras-Esquivel, Juan C; Gutiérrez-Sánchez, Gerardo; Aguilar, Cristóbal N

2017-09-01

Pomegranate-husk is the main by-product generated from the pomegranate industry. It is a potential source of compounds highly appreciated by different costumers. Punicalagin is the main compound present in pomegranate-husk. To characterise the pomegranate-husk total polyphenols by HPLC-ESI-MS and to establish a method for the recovery of punicalagin using a medium pressure liquid chromatography (MPLC) system. The characterisation of total pomegranate-husk polyphenols was carried out using liquid chromatography coupled to mass spectrometry. Thus, 200 mg of pomegranate-husk polyphenols were fractionated by MPLC. The isolated punicalagin was characterised by HPLC-MS and was tested as standard reagent for the measurement of its scavenging capacity reducing DPPH and ABTS radicals. Twenty peaks were identified by analytical HPLC-MS analysis from the pomegranate-husk polyphenols. The main compounds were the punicalagin anomers, punicalin and ellagic acid. The MPLC method allowed three fractions to be obtained. In fraction three 39.40 ± 8.06 mg of punicalagin anomers (purity > 97.9%) were recovered. The scavenging capacity of punicalagin showed an IC 50 of 109.53 and 151.50 μg/mL for DPPH and ABTS radicals, respectively. The MPLC system was an excellent tool for the separation of the main ellagitannins from pomegranate husk and for the isolation of punicalagin anomers. Fraction three was rich in high purity punicalagin anomers. The IC 50 was obtained for DPPH and ABTS radicals. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Method for preparing actinide nitrides

DOEpatents

Bryan, G.H.; Cleveland, J.M.; Heiple, C.R.

1975-12-01

Actinide nitrides, and particularly plutonium and uranium nitrides, are prepared by reacting an ammonia solution of an actinide compound with an ammonia solution of a reactant or reductant metal, to form finely divided actinide nitride precipitate which may then be appropriately separated from the solution. The actinide nitride precipitate is particularly suitable for forming nuclear fuels.

Dzyaloshinskii-Moriya interaction and magnetic anisotropies in Uranium compounds

NASA Astrophysics Data System (ADS)

Sandratskii, L. M.

2018-05-01

We report on the first-principles study of complex noncollinear magnetic structures in Uranium compounds. We contrast two cases. The first is the periodic magnetic structure of U2Pd2In with exactly orthogonal atomic moments, the second is an incommensurate plane spiral structure of UPtGe where the angle between atomic moments of nearest neighbors is also close to 90°. We demonstrate that the hierarchy of magnetic interactions leading to the formation of the magnetic structure is opposite in the two cases. In U2Pd2In, the magnetic anisotropy plays the leading role, followed by the Dzyaloshinskii-Moriya interaction (DMI) interaction specifying the chirality of the structure. Here, the interatomic exchange interaction does not play important role. In UPtGe the hierarchy of the interactions is opposite. The leading interaction is the interatomic exchange interaction responsible for the formation of the incommensurate spiral structure followed by the DMI responsible for the selected chirality of the helix. The magnetic anisotropy is very weak that is a prerequisite for keeping the distortion of the helical structure weak.

Method of isotope separation by chemi-ionization

DOEpatents

Wexler, Sol; Young, Charles E.

1977-05-17

A method for separating specific isotopes present in an isotopic mixture by aerodynamically accelerating a gaseous compound to form a jet of molecules, and passing the jet through a stream of electron donor atoms whereby an electron transfer takes place, thus forming negative ions of the molecules. The molecular ions are then passed through a radiofrequency quadrupole mass filter to separate the specific isotopes. This method may be used for any compounds having a sufficiently high electron affinity to permit negative ion formation, and is especially useful for the separation of plutonium and uranium isotopes.

Investigation of Strain Aging in the Ordered Intermetallic Compound beta-NiAl. Ph.D. Thesis Final Contractor Report

NASA Technical Reports Server (NTRS)

Weaver, Mark Lovell

1995-01-01

The phenomenon of strain aging has been investigated in polycrystalline and single crystal NiAl alloys at temperatures between 300 and 1200 K. Static strain aging studies revealed that after annealing at 1100 K for 7200 s (i.e., 2h) followed by furnace cooling, high purity, nitrogen-doped and titanium-doped polycrystalline alloys exhibited continuous yielding, while conventional-purity and carbon-doped alloys exhibited distinct yield points and Luders strains. Prestraining by hydrostatic pressurization removed the yield points, but they could be reintroduced by further annealing treatments. Yield points could be reintroduced more rapidly if the specimens were prestrained uniaxially rather than hydrostatically, owing to the arrangement of dislocations into cell structures during uniaxial deformation. The time dependence of the strain aging events followed at t(exp 2/3) relationship suggesting that the yield points observed in polycrystalline NiAl were the result of the pinning of mobile dislocations by interstitials, specifically carbon. Between 700 and 800 K, yield stress plateaus, yield stress transients upon a ten-fold increase in strain rate, work hardening peaks, and dips in the strain rate sensitivity (SRS) have been observed in conventional-purity and carbon-doped polycrystals. In single crystals, similar behavior was observed; in conventional-purity single crystals, however, the strain rate sensitivity became negative resulting in serrated yielding, whereas, the strain rate sensitivity stayed positive in high purity and in molybdenum-doped NiAl. These observations are indicative of dynamic strain aging (DSA) and are discussed in terms of conventional strain aging theories. The impact of these phenomena on the composition-structure-property relations are discerned. Finally, a good correlation has been demonstrated between the properties of NiAl alloys and a recently developed model for strain aging in metals and alloys developed by Reed-Hill et al.

Geological conditions of safe long-term storage and disposal of depleted uranium hexafluoride

NASA Astrophysics Data System (ADS)

Laverov, N. P.; Velichkin, V. I.; Omel'Yanenko, B. I.; Yudintsev, S. V.; Tagirov, B. R.

2010-08-01

The production of enriched uranium used in nuclear weapons and fuel for atomic power plants is accompanied by the formation of depleted uranium (DU), the amount of which annually increases by 35-40 kt. To date, more than 1.6 Mt DU has accumulated in the world. The main DU mass is stored as environ-mentally hazardous uranium hexafluoride (UF6), which is highly volatile and soluble in water with the formation of hydrofluoric acid. To ensure safe UF6 storage, it is necessary to convert this compound in chemically stable phases. The industrial reprocessing of UF6 into U3O8 and HF implemented in France is highly expensive. We substantiate the expediency of long-term storage of depleted uranium hexafluoride in underground repositories localized in limestone. On the basis of geochemical data and thermodynamic calculations, we show that interaction in the steel container-UF6-limestone-groundwater system gives rise to the development of a slightly alkaline reductive medium favorable for chemical reaction with formation of uraninite (UO2) and fluorite (CaF2). The proposed engineering solution not only ensures safe DU storage but also makes it possible to produce uraninite, which can be utilized, if necessary, in fast-neutron reactors. In the course of further investigations aimed at safe maintenance of DU, it is necessary to study the kinetics of conversion of UF6 into stable phases, involving laboratory and field experiments.

The phase state at high temperatures in the MOX-SiO 2 system

NASA Astrophysics Data System (ADS)

Nakamichi, S.; Kato, M.; Sunaoshi, T.; Uchida, T.; Morimoto, K.; Kashimura, M.; Kihara, Y.

2009-06-01

Influence of impurity Si on microstructure in a plutonium and uranium mixed oxide (MOX), which is used for fast breeder reactor fuel, was investigated, and phase state in 25% SiO 2 - (U 0.7Pu 0.3)O 2 was observed as a function of oxygen chemical potential. Compounds composed of Pu and Si with other elements were observed at grain boundaries of the MOX parent phase in the specimens after annealing. These compounds were not observed in the grain interior and the MOX phase was not affected significantly by impurity Si. It was found that the compounds tended to form more observably with decreasing O/M ratio and with increasing annealing temperatures.

Formation of natural indigo derived from woad (Isatis tinctoria L.) in relation to product purity.

PubMed

Garcia-Macias, Paulina; John, Philip

2004-12-29

There is an increasing commercial demand for naturally sourced indigo that meets the purity standards set by the synthetic product. This study concerns the indigo made from leaves of woad (Isatis tinctoria L.), and in particular its interaction with particulate impurities arising from soil and plant materials. Also, a more reliable method using N-methyl-2-pyrrolidone has been developed for the spectrophotometric determination of indigo. In a novel application of fluorescence spectroscopy, indoxyl intermediates in indigo formation are shown to be stable for minutes. The main indigo precursor from woad can be adsorbed onto Amberlite XAD16 in conformity with a Langmuir isotherm, but indigo precursors break down on this and other resin beads to yield indigo and red compounds. Indigo made from indoxyl acetate aggregates into particles, the size distribution of which can be modified by the inclusion of a fine dispersion of calcium hydroxide. Bright field microscopy of indigo products made under defined conditions and scanning electron microscopy combined with energy-dispersive X-ray analysis reveal the relationship of indigo with particulate materials. A model illustrating the interaction of indigo with particulate contaminants is developed on the basis of the results obtained, and recommendations are made for improving the purity of natural indigo.

Preparation and Stoichiometry Effects on Microstructure and Properties of High Purity BaTiO3.

DTIC Science & Technology

1986-03-27

oxalate , citrate) salt solutions, from mixed alkoxide precursors or from hydrothermal solutions. Typical starting materials and reaction sequences...decomposition and calcination reactions to form the BaTiO compound. Both the oxalate and 3 hydrothermal processes show commnercial promise and are briefly...thermal decomposition of oxalates and by hydrothermal synthesis. As-received lots of mixed oxide and oxalate -derived powders had Ba:TI ratios of 0.997 and

Solid state speciation of uranium and its local structure in Sr2CeO4 using photoluminescence spectroscopy.

PubMed

Sahu, M; Gupta, Santosh K; Jain, D; Saxena, M K; Kadam, R M

2018-04-15

An effort was taken to carry our speciation study of uranium ion in technologically important cerate host Sr 2 CeO 4 using time resolved photoluminescence spectroscopy. Such studies are not relevant only to nuclear industry but can give rich insight into fundamentals of 5f electron chemistry in solid state systems. In this work both undoped and varied amount of uranium doped Sr 2 CeO 4 compound is synthesized using complex polymerization method and is characterized systematically using X-ray diffraction (XRD), Raman spectroscopy, impedance spectroscopy and scanning electron microscopy (SEM). Both XRD and Raman spectroscopy confirmed the formation of pure Sr 2 CeO 4 which has tendency to decompose peritectically to SrCeO 3 and SrO at higher temperature. Uranium doping is confirmed by XRD. Uranium exhibits a rich chemistry owing to its variable oxidation state from +3 to +6. Each of them exhibits distinct luminescence properties either due to f-f transitions or ligand to metal charge transfer (LMCT). We have taken Sr 2 CeO 4 as a model host lattice to understand the photophysical characteristics of uranium ion in it. Emission spectroscopy revealed the stabilization of uranium as U (VI) in the form of UO 6 6- (octahedral uranate) in Sr 2 CeO 4 . Emission kinetics study reflects that uranate ions are not homogeneously distributed in Sr 2 CeO 4 and it has two different environments due to its stabilization at both Sr 2+ as well as Ce 4+ site. The lifetime population analysis interestingly pinpointed that majority of uranate ion resided at Ce 4+ site. The critical energy-transfer distance between the uranate ion was determined based on which the concentration quenching mechanism was attributed to electric multipolar interaction. These studies are very important in designing Sr 2 CeO 4 based optoelectronic material as well exploring it for actinides studies. Copyright © 2018 Elsevier B.V. All rights reserved.

Properties, use and health effects of depleted uranium (DU): a general overview.

PubMed

Bleise, A; Danesi, P R; Burkart, W

2003-01-01

Depleted uranium (DU), a waste product of uranium enrichment, has several civilian and military applications. It was used as armor-piercing ammunition in international military conflicts and was claimed to contribute to health problems, known as the Gulf War Syndrome and recently as the Balkan Syndrome. This led to renewed efforts to assess the environmental consequences and the health impact of the use of DU. The radiological and chemical properties of DU can be compared to those of natural uranium, which is ubiquitously present in soil at a typical concentration of 3 mg/kg. Natural uranium has the same chemotoxicity, but its radiotoxicity is 60% higher. Due to the low specific radioactivity and the dominance of alpha-radiation no acute risk is attributed to external exposure to DU. The major risk is DU dust, generated when DU ammunition hits hard targets. Depending on aerosol speciation, inhalation may lead to a protracted exposure of the lung and other organs. After deposition on the ground, resuspension can take place if the DU containing particle size is sufficiently small. However, transfer to drinking water or locally produced food has little potential to lead to significant exposures to DU. Since poor solubility of uranium compounds and lack of information on speciation precludes the use of radioecological models for exposure assessment, biomonitoring has to be used for assessing exposed persons. Urine, feces, hair and nails record recent exposures to DU. With the exception of crews of military vehicles having been hit by DU penetrators, no body burdens above the range of values for natural uranium have been found. Therefore, observable health effects are not expected and residual cancer risk estimates have to be based on theoretical considerations. They appear to be very minor for all post-conflict situations, i.e. a fraction of those expected from natural radiation.

Solid state speciation of uranium and its local structure in Sr2CeO4 using photoluminescence spectroscopy

NASA Astrophysics Data System (ADS)

Sahu, M.; Gupta, Santosh K.; Jain, D.; Saxena, M. K.; Kadam, R. M.

2018-04-01

An effort was taken to carry our speciation study of uranium ion in technologically important cerate host Sr2CeO4 using time resolved photoluminescence spectroscopy. Such studies are not relevant only to nuclear industry but can give rich insight into fundamentals of 5f electron chemistry in solid state systems. In this work both undoped and varied amount of uranium doped Sr2CeO4 compound is synthesized using complex polymerization method and is characterized systematically using X-ray diffraction (XRD), Raman spectroscopy, photoluminescence spectroscopy and scanning electron microscopy (SEM). Both XRD and Raman spectroscopy confirmed the formation of pure Sr2CeO4 which has tendency to decompose peritectically to SrCeO3 and SrO at higher temperature. Uranium doping is confirmed by XRD. Uranium exhibits a rich chemistry owing to its variable oxidation state from +3 to +6. Each of them exhibits distinct luminescence properties either due to f-f transitions or ligand to metal charge transfer (LMCT). We have taken Sr2CeO4 as a model host lattice to understand the photophysical characteristics of uranium ion in it. Emission spectroscopy revealed the stabilization of uranium as U (VI) in the form of UO66- (octahedral uranate) in Sr2CeO4. Emission kinetics study reflects that uranate ions are not homogeneously distributed in Sr2CeO4 and it has two different environments due to its stabilization at both Sr2+ as well as Ce4+ site. The lifetime population analysis interestingly pinpointed that majority of uranate ion resided at Ce4+ site. The critical energy-transfer distance between the uranate ion was determined based on which the concentration quenching mechanism was attributed to electric multipolar interaction. These studies are very important in designing Sr2CeO4 based optoelectronic material as well exploring it for actinides studies.

Porous Materials for Hydrolytic Dehydrogenation of Ammonia Borane

PubMed Central

Umegaki, Tetsuo; Xu, Qiang; Kojima, Yoshiyuki

2015-01-01

Hydrogen storage is still one of the most significant issues hindering the development of a “hydrogen energy economy”. Ammonia borane is notable for its high hydrogen densities. For the material, one of the main challenges is to release efficiently the maximum amount of the stored hydrogen. Hydrolysis reaction is a promising process by which hydrogen can be easily generated from this compound. High purity hydrogen from this compound can be evolved in the presence of solid acid or metal based catalyst. The reaction performance depends on the morphology and/or structure of these materials. In this review, we survey the research on nanostructured materials, especially porous materials for hydrogen generation from hydrolysis of ammonia borane. PMID:28793453

Uranium reduction and microbial community development in response to stimulation with different electron donors.

PubMed

Barlett, Melissa; Moon, Hee Sun; Peacock, Aaron A; Hedrick, David B; Williams, Kenneth H; Long, Philip E; Lovley, Derek; Jaffe, Peter R

2012-07-01

Stimulating microbial reduction of soluble U(VI) to less soluble U(IV) shows promise as an in situ bioremediation strategy for uranium contaminated groundwater, but the optimal electron donors for promoting this process have yet to be identified. The purpose of this study was to better understand how the addition of various electron donors to uranium-contaminated subsurface sediments affected U(VI) reduction and the composition of the microbial community. The simple electron donors, acetate or lactate, or the more complex donors, hydrogen-release compound (HRC) or vegetable oil, were added to the sediments incubated in flow-through columns. The composition of the microbial communities was evaluated with quantitative PCR probing specific 16S rRNA genes and functional genes, phospholipid fatty acid analysis, and clone libraries. All the electron donors promoted U(VI) removal, even though the composition of the microbial communities was different with each donor. In general, the overall biomass, rather than the specific bacterial species, was the factor most related to U(VI) removal. Vegetable oil and HRC were more effective in stimulating U(VI) removal than acetate. These results suggest that the addition of more complex organic electron donors could be an excellent option for in situ bioremediation of uranium-contaminated groundwater.

Purification of coumarin compounds from Cortex fraxinus by adsorption chromatography.

PubMed

Yu, Minglan; Sun, Ailing; Zhang, Yongqing; Liu, Renmin

2014-10-01

In this paper, a chromatographic method for isolation and purification of coumarin compounds from Cortex fraxinus was established by using Superose 12 as the separation media for the first time. The conditions for separation were optimized. Four kinds of coumarin compounds including aesuletin, aesculin, fraxetin and fraxin were obtained. The purity of these compounds were 98.5, 99.1, 97.9 and 97.3%, respectively, which were determined by HPLC area normalization method. The chemical structures of the separated compounds were identified according to (1)H and (13)C nuclear magnetic resonance data. The retention behavior of the separated coumarin compounds on Superose 12 was also discussed. The retention is based on a mixture of hydrogen bonding and hydrophobic interactions between the coumarin compounds and the residues of the cross-linking reagents used in the manufacturing process of Superose 12. The results of this paper indicate that Superose 12 is not only suitable for size-exclusion chromatography of proteins and other biological macromolecules but also for low-molecular-weight natural products. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

U.S. Food and Drug Administration Inspections: Guide to a Successful Outcome for 503A Sterile Compounding Pharmacies.

PubMed

Yoch, Doug

2017-01-01

The reasons for which pharmaceutical compounding is the focus of intense state and federal scrutiny are now well known. Compounders are faced with an ever-increasing need to prove, by objective standards, the safety, purity, and potency of the formulations they dispense. They must also demonstrate their compliance with regulations often based on current good compounding practices designed for the pharmaceutical industry. In the U.S. today, rigorous unannounced state and federal inspections of compounding facilities are occurring more and more frequently. To achieve a successful outcome, communicating clearly and effectively with inspectors and having ready access to the information they request are as critical as proving compliance. This article describes the author's experience with an unannounced United States Food and Drug Administration inspection of his 503A compounding facility and his response to the findings. Readers will learn what to expect during such an inspection, how to prepare for that event, and how to achieve an excellent outcome. Those who would like more information about any of the topics presented are invited to contact the author at the address provided at the close of this article. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Unexpected Magnetic Ordering on the Cr Substructure in UCr2Si2C and Structural Relationships in Quaternary U-Cr-Si-C Compounds.

PubMed

Lemoine, Pierric; Vernière, Anne; Pasturel, Mathieu; Venturini, Gérard; Malaman, Bernard

2018-03-05

Previous experimental and theoretical studies revealed that carbon insertion into the RCr 2 Si 2 compounds drastically affects the magnetic behavior, since chromium does not carry any magnetic moment in RCr 2 Si 2 C (R = Y, La-Sm, Gd-Er) compounds in contrast to RCr 2 Si 2 (R = Y, Sm, Gd-Lu, Th) compounds. In this study, we report on the unexpected magnetic ordering of chromium atoms in the isotype quaternary UCr 2 Si 2 C compound. While specific heat and magnetic measurements suggest a Pauli paramagnetic behavior, neutron powder diffraction reveals an antiferromagnetic ordering of the chromium substructure at high temperature ( T N > 300 K), while that of uranium remains nonmagnetically ordered down to 2 K. Its magnetic behavior, inverse in comparison to the RCr 2 Si 2 C carbides involving a magnetic lanthanide, is discussed in relation with the singularity of its crystal structure among the series. Moreover, the crystallographic structures and the structural stability of UCr 2 Si 2 C and of two other quaternary U-Cr-Si-C compounds (i.e., UCr 3 Si 2 C and U 2 Cr 3 Si 2 C 3 ), based on the full occupancy of interstitial sites by carbon atoms, are discussed and compared to those of the related ternary intermetallics. Finally, the low-temperature form of UCr 2 Si 2 , corresponding to a displacive transformation around 210 K of the ThCr 2 Si 2 -type structure, is reinvestigated by considering a higher symmetry monoclinic unit cell ( C2/ m) instead of the previously reported triclinic cell ( P1̅). The antiferromagnetic ordering at low temperature ( T N = 30(2) K) of the uranium substructure is confirmed, and its magnetic structure is reanalyzed and discussed considering the monoclinic crystal structure.

Separation and purification of polyphenols from red wine extracts using high speed counter current chromatography.

PubMed

Li, Yuanyuan; Li, Lingxi; Cui, Yan; Zhang, Shuting; Sun, Baoshan

2017-06-01

Polyphenols are important compounds of red wine owing to their contribution to sensory properties and antioxidant activities. In this study, high-speed counter-current chromatography (HSCCC) coupled with semi-preparative HPLC was used for large-scale separation and purification of polyphenols from red wine extracts. With the solvent system of hexane-ethyl acetate-water (1-50-50), various oligomeric procyanidins including monomer catechin, epicatechin, dimers B1, B2; phenolic acids including coutaric acid, caftaric acid and other type of polyphenols were largely separated within 370min and most of these compounds presented high yields (0.97mg to 13.79mg) with high purity (90.34% to 98.91%) after the semi-preparative HPLC isolation. Using the solvent system of Methyl tert-Butyl Ether (MTBE) - n-butyl alcohol- acetonitrile-water (1-40-1-50, acidified with 0.01% trifluoroacetic acid (TFA)) by one-step HSCCC of 100mg of the red wine extracts, the major anthocyanins, i.e., malvidin-3-O-glucoside, delphinidin-3-O-glucoside and peonidin-3-O-glucoside, as well as two polymeric proanthocyanidin fractions were successfully separated one another within 320min. The yields of malvidin-3-O-glucoside, delphinidin-3-O-glucoside and peonidin-3-O-glucoside were 12.12mg, 1.78mg and 11.57mg with the purity of 92.74%, 91.03% and 91.21%, respectively. Thiolysis-UPLC analysis indicated that the two polymeric proanthocyanidin fractions presented high purity, with mean degree of polymerization of 7.66±0.12 and 6.20±0.09, respectively. The further experiments on the antioxidant activities by DPPH radical test, FRAP assay and ABTS method showed that all of the isolated procyandins and anthocyanins and the two polymeric proanthocyanidin fractions, with exception of phenolic acids possessed much greater antioxidant activities compared to standard Trolox andl-ascorbic acid (2-14 times). Copyright © 2017 Elsevier B.V. All rights reserved.

cis,cis-Muconic acid: separation and catalysis to bio-adipic acid for nylon-6,6 polymerization

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

Vardon, Derek R.; Rorrer, Nicholas A.; Salvachúa, Davinia

cis,cis-Muconic acid is a polyunsaturated dicarboxylic acid that can be produced renewably via the biological conversion of sugars and lignin-derived aromatic compounds. Subsequently, muconic acid can be catalytically converted to adipic acid -- the most commercially significant dicarboxylic acid manufactured from petroleum. Nylon-6,6 is the major industrial application for adipic acid, consuming 85% of market demand; however, high purity adipic acid (99.8%) is required for polymer synthesis. As such, process technologies are needed to effectively separate and catalytically transform biologically derived muconic acid to adipic acid in high purity over stable catalytic materials. To that end, this study: (1) demonstratesmore » bioreactor production of muconate at 34.5 g L-1 in an engineered strain of Pseudomonas putida KT2440, (2) examines the staged recovery of muconic acid from culture media, (3) screens platinum group metals (e.g., Pd, Pt, Rh, Ru) for activity and leaching stability on activated carbon (AC) and silica supports, (4) evaluates the time-on-stream performance of Rh/AC in a trickle bed reactor, and (5) demonstrates the polymerization of bio-adipic acid to nylon-6,6. Separation experiments confirmed AC effectively removed broth color compounds, but subsequent pH/temperature shift crystallization resulted in significant levels of Na, P, K, S and N in the crystallized product. Ethanol dissolution of muconic acid precipitated bulk salts, achieving a purity of 99.8%. Batch catalysis screening reactions determined that Rh and Pd were both highly active compared to Pt and Ru, but Pd leached significantly (1-9%) from both AC and silica supports. Testing of Rh/AC in a continuous trickle bed reactor for 100 h confirmed stable performance after 24 h, although organic adsorption resulted in reduced steady-state activity. Lastly, polymerization of bio-adipic acid with hexamethyldiamine produced nylon-6,6 with comparable properties to its petrochemical counterpart, thereby demonstrating a path towards bio-based nylon production via muconic acid.« less

Assessment of Radioactive Materials and Heavy Metals in the Surface Soil around the Bayanwula Prospective Uranium Mining Area in China

PubMed Central

Bai, Haribala; Hu, Bitao; Wang, Chengguo; Bao, Shanhu; Sai, Gerilemandahu; Xu, Xiao; Zhang, Shuai; Li, Yuhong

2017-01-01

The present work is the first systematic and large scale study on radioactive materials and heavy metals in surface soil around the Bayanwula prospective uranium mining area in China. In this work, both natural and anthropogenic radionuclides and heavy metals in 48 surface soil samples were analyzed using High Purity Germanium (HPGe) γ spectrometry and inductively coupled plasma-mass spectrometry (ICP-MS). The obtained mean activity concentrations of 238U, 226Ra, 232Th, 40K, and 137Cs were 25.81 ± 9.58, 24.85 ± 2.77, 29.40 ± 3.14, 923.0 ± 47.2, and 5.64 ± 4.56 Bq/kg, respectively. The estimated average absorbed dose rate and annual effective dose rate were 76.7 ± 3.1 nGy/h and 83.1 ± 3.8 μSv, respectively. The radium equivalent activity, external hazard index, and internal hazard index were also calculated, and their mean values were within the acceptable limits. The estimated lifetime cancer risk was 3.2 × 10−4/Sv. The heavy metal contents of Cr, Ni, Cu, Zn, As, Cd, and Pb from the surface soil samples were measured and their health risks were then assessed. The concentrations of all heavy metals were much lower than the average backgrounds in China except for lead which was about three times higher than that of China’s mean. The non-cancer and cancer risks from the heavy metals were estimated, which are all within the acceptable ranges. In addition, the correlations between the radionuclides and the heavy metals in surface soil samples were determined by the Pearson linear coefficient. Strong positive correlations between radionuclides and the heavy metals at the 0.01 significance level were found. In conclusion, the contents of radionuclides and heavy metals in surface soil around the Bayanwula prospective uranium mining area are at a normal level. PMID:28335450

Assessment of Radioactive Materials and Heavy Metals in the Surface Soil around the Bayanwula Prospective Uranium Mining Area in China.

PubMed

Bai, Haribala; Hu, Bitao; Wang, Chengguo; Bao, Shanhu; Sai, Gerilemandahu; Xu, Xiao; Zhang, Shuai; Li, Yuhong

2017-03-14

The present work is the first systematic and large scale study on radioactive materials and heavy metals in surface soil around the Bayanwula prospective uranium mining area in China. In this work, both natural and anthropogenic radionuclides and heavy metals in 48 surface soil samples were analyzed using High Purity Germanium (HPGe) γ spectrometry and inductively coupled plasma-mass spectrometry (ICP-MS). The obtained mean activity concentrations of 238 U, 226 Ra, 232 Th, 40 K, and 137 Cs were 25.81 ± 9.58, 24.85 ± 2.77, 29.40 ± 3.14, 923.0 ± 47.2, and 5.64 ± 4.56 Bq/kg, respectively. The estimated average absorbed dose rate and annual effective dose rate were 76.7 ± 3.1 nGy/h and 83.1 ± 3.8 μ Sv, respectively. The radium equivalent activity, external hazard index, and internal hazard index were also calculated, and their mean values were within the acceptable limits. The estimated lifetime cancer risk was 3.2 × 10 -4 /Sv. The heavy metal contents of Cr, Ni, Cu, Zn, As, Cd, and Pb from the surface soil samples were measured and their health risks were then assessed. The concentrations of all heavy metals were much lower than the average backgrounds in China except for lead which was about three times higher than that of China's mean. The non-cancer and cancer risks from the heavy metals were estimated, which are all within the acceptable ranges. In addition, the correlations between the radionuclides and the heavy metals in surface soil samples were determined by the Pearson linear coefficient. Strong positive correlations between radionuclides and the heavy metals at the 0.01 significance level were found. In conclusion, the contents of radionuclides and heavy metals in surface soil around the Bayanwula prospective uranium mining area are at a normal level.

Separation of five compounds from leaves of Andrographis paniculata (Burm. f.) Nees by off-line two-dimensional high-speed counter-current chromatography combined with gradient and recycling elution.

PubMed

Zhang, Li; Liu, Qi; Yu, Jingang; Zeng, Hualiang; Jiang, Shujing; Chen, Xiaoqing

2015-05-01

An off-line two-dimensional high-speed counter-current chromatography method combined with gradient and recycling elution mode was established to isolate terpenoids and flavones from the leaves of Andrographis paniculata (Burm. f.) Nees. By using the solvent systems composed of n-hexane/ethyl acetate/methanol/water with different volume ratios, five compounds including roseooside, 5,4'-dihydroxyflavonoid-7-O-β-d-pyranglucuronatebutylester, 7,8-dimethoxy-2'-hydroxy-5-O-β-d-glucopyranosyloxyflavon, 14-deoxyandrographiside, and andrographolide were successfully isolated. Purities of these isolated compounds were all over 95% as determined by high-performance liquid chromatography. Their structures were identified by UV, mass spectrometry, and (1) H NMR spectroscopy. It has been demonstrated that the combination of off-line two-dimensional high-speed counter-current chromatography with different elution modes is an efficient technique to isolate compounds from complex natural product extracts. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and in vitro evaluation of new derivatives of 2-substituted-6-fluorobenzo[d]thiazoles as cholinesterase inhibitors.

PubMed

Imramovský, Aleš; Pejchal, Vladimír; Štěpánková, Šárka; Vorčáková, Katarína; Jampílek, Josef; Vančo, Ján; Šimůnek, Petr; Královec, Karel; Brůčková, Lenka; Mandíková, Jana; Trejtnar, František

2013-04-01

A series of novel cholinesterase inhibitors based on 2-substituted 6-fluorobenzo[d]thiazole were synthesised and characterised by IR, (1)H, (13)C and (19)F NMR spectroscopy and HRMS. Purity was checked by elemental analyses. The novel carbamates were tested for their ability to inhibit acetylcholinesterase (AChE) and butyrylcholinesterase (BChE). The toxicity of the most active compounds was investigated using a standard in vitro test with HepG2 cells, and the ratio between biological activity and toxicity was determined. In addition, the toxicity of the most active compounds was evaluated against MCF7 cells using the xCELLigence system. Structure-activity relationships reflecting the dependence of cholinesterase inhibitors on the lipophilicity of the compounds as well as on the Taft polar and steric substituent constants are discussed. The specific orientation of the inhibitors in the binding site of acetylcholinesterase was determined using molecular docking of the most active compound. Copyright © 2013 Elsevier Ltd. All rights reserved.

Regioselective and stereospecific deuteration of bioactive aza compounds by the use of ruthenium nanoparticles.

PubMed

Pieters, Grégory; Taglang, Céline; Bonnefille, Eric; Gutmann, Torsten; Puente, Céline; Berthet, Jean-Claude; Dugave, Christophe; Chaudret, Bruno; Rousseau, Bernard

2014-01-03

An efficient H/D exchange method allowing the deuteration of pyridines, quinolines, indoles, and alkyl amines with D2 in the presence of Ru@PVP nanoparticles is described. By a general and simple procedure involving mild reaction conditions and simple filtration to recover the labeled product, the isotopic labeling of 22 compounds proceeded in good yield with high chemo- and regioselectivity. The viability of this procedure was demonstrated by the labeling of eight biologically active compounds. Remarkably, enantiomeric purity was conserved in the labeled compounds, even though labeling took place in the vicinity of the stereogenic center. The level of isotopic enrichment observed is suitable for metabolomic studies in most cases. This approach is also perfectly adapted to tritium labeling because it uses a gas as an isotopic source. Besides these applications to molecules of biological interest, this study reveals a rich and underestimated chemistry on the surface of ruthenium nanoparticles. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chloro-, methyl-, and (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV) and -uranium(IV). Crystal structure of (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV)

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

Turner, H.W.; Andersen, R.A.; Zalkin, A.

1979-05-01

Reaction of sodium (hexamethyldisilyl)amide with thorium tetrachloride or uranium tetrachloride yields chlorotris-((hexamethyldisilyl)amido)thorium(IV) or -uranium(IV), respectively. The chloroamides of thorium or uranium react with dimethylmagnesium or methyllithium yielding the methyl derivatives MeTh(N(SiMe/sub 3/)/sub 2/)/sub 3/ or MeU(N(SiMe/sub 3/)/sub 2/)/sub 3/, respectively. The chloro compounds yield BH/sub 4/M(N(SiMe/sub 3/)/sub 2/)/sub 3/ upon reaction with lithium tetrahydroborate, where M is thorium or uranium. Infrared spectra of the tetrahydroborate derivatives suggest that BH/sub 4/ is bonded in a tridentate fashion in both compounds, the metal atoms being six-coordinate. Single-crystal X-ray analysis of the thorium borohydride confirms the infrared result. The white BH/sub 4/Th(N(Si(CH/sub 3/))/submore » 2/)/sub 3/ crystals are rhombohedral with cell dimensions a/sub r/ = 11.137 A and ..cap alpha../sub r/ = 113.61/sup 0/; the triply primitive hexagonal cell has a/sub h/ = 18.640 (3) A c/sub h/ = 8.604 (1) A, V = 2489 A/sup 3/, Z = 3, and D/sub x/ = 1.40 g/cm/sup 3/, space group R3m. The structure was refined by full-matrix least squares to a conventional R factor of 0.031 for 1014 data. The Th atom is on a threefold axis 2.32 A from three nitrogen atoms and 2.61 A from the boron atom, a distance which represents a triple bridge bond between Th and B. The three (dimethylsilyl)amide ligands are disordered by a mirror plane parallel to the threefold axis. CH/sub 3/Th(N(Si(CH/sub 3/)/sub 3/)/sub 2/)/sub 3/ is isomorphous with BH/sub 4/Th(N(Si(CH/sub 3/)/sub 3/)/sub 2/)/sub 3/ with cell dimensions a/sub h/ = 18.68 (1) A and c/sub h/ = 8.537 (6) A. The diffraction data yielded integral'' = 12.16 +- 0.33 e for the imaginary scattering term for Th with Cu K..cap alpha.. radiation.« less

Novel 2-step synthetic indole compound 1,1,3-tri(3-indolyl)cyclohexane inhibits cancer cell growth in lung cancer cells and xenograft models.

PubMed

Lee, Ching-Hsiao; Yao, Ching-Fa; Huang, Sin-Ming; Ko, Shengkai; Tan, Yi-Hung; Lee-Chen, Guey-Jen; Wang, Yi-Ching

2008-08-15

The clinical responses to chemotherapy in lung cancer patients are unsatisfactory. Thus, the development of more effective anticancer drugs for lung cancer is urgently needed. A 2-step novel synthetic compound, referred to as 1,1,3-tri(3-indolyl)cyclohexane (3-indole), was generated in high purity and yield. 3-Indole was tested for its biologic activity in A549, H1299, H1435, CL1-1, and H1437 lung cancer cells. Animal studies were also performed. The data indicate that 3-indole induced apoptosis in various lung cancer cells. Increased cytochrome-c release from mitochondria to cytosol, decreased expression of antiapoptotic Bcl-2, and increased expression of proapoptotic Bax were observed. In addition, 3-indole stimulated caspases-3, -9, and to a lesser extent caspase-8 activities in cancer cells, suggesting that the intrinsic mitochondria pathway was the potential mechanism involved in 3-indole-induced apoptosis. 3-Indole-induced a concentration-dependent mitochondrial membrane potential dissipation and an increase in reactive oxygen species (ROS) production. Activation of c-Jun N-terminal kinase (JNK) and triggering of DNA damage were also apparent. Note that 3-indole-induced JNK activation and DNA damage can be partially suppressed by an ROS inhibitor. Apoptosis induced by 3-indole could be abrogated by ROS or JNK inhibitors, suggesting the importance of ROS and JNK stress-related pathways in 3-indole-induced apoptosis. Moreover, 3-indole showed in vivo antitumor activities against human xenografts in murine models. On the basis of its potent anticancer activity in cell and animal models, the data suggest that this 2-step synthetic 3-indole compound of high purity and yield is a potential candidate to be tested as a lead pharmaceutical compound for cancer treatment. 2008 American Cancer Society

High-throughput screening of a diversity collection using biodefense category A and B priority pathogens.

PubMed

Barrow, Esther W; Clinkenbeard, Patricia A; Duncan-Decocq, Rebecca A; Perteet, Rachel F; Hill, Kimberly D; Bourne, Philip C; Valderas, Michelle W; Bourne, Christina R; Clarkson, Nicole L; Clinkenbeard, Kenneth D; Barrow, William W

2012-08-01

One of the objectives of the National Institutes of Allergy and Infectious Diseases (NIAID) Biodefense Program is to identify or develop broad-spectrum antimicrobials for use against bioterrorism pathogens and emerging infectious agents. As a part of that program, our institution has screened the 10 000-compound MyriaScreen Diversity Collection of high-purity druglike compounds against three NIAID category A and one category B priority pathogens in an effort to identify potential compound classes for further drug development. The effective use of a Clinical and Laboratory Standards Institute-based high-throughput screening (HTS) 96-well-based format allowed for the identification of 49 compounds that had in vitro activity against all four pathogens with minimum inhibitory concentration values of ≤16 µg/mL. Adaptation of the HTS process was necessary to conduct the work in higher-level containment, in this case, biosafety level 3. Examination of chemical scaffolds shared by some of the 49 compounds and assessment of available chemical databases indicates that several may represent broad-spectrum antimicrobials whose activity is based on novel mechanisms of action.

SEPARATION PROCESS FOR ZIRCONIUM AND COMPOUNDS THEREOF

DOEpatents

Crandall, H.W.; Thomas, J.R.

1959-06-30

The separation of zirconium from columbium, rare earths, yttrium and the alkaline earth metals, such mixtures of elements occurring in zirconium ores or neutron irradiated uranium is described. According to the invention a suitable separation of zirconium from a one normal acidic aqueous solution containing salts, nitrates for example, of tetravalent zirconium, pentavalent columbium, yttrium, rare earths in the trivalent state and alkaline earths can be obtained by contacting the aqueous solution with a fluorinated beta diketonc alone or in an organic solvent solution, such as benzene, to form a zirconium chelate compound. When the organic solvent is present the zirconium chelate compound is directly extracted; otherwise it is separated by filtration. The zirconium may be recovered from contacting the organic solvent solution containing the chelated compound by back extraction with either an aqueous hydrofluoric acid or an oxalic acid solution.

Potential Signatures of Semi-volatile Compounds Associated With Nuclear Processing

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

Probasco, Kathleen M.; Birnbaum, Jerome C.; Maughan, A. D.

2002-06-01

Semi-volatile chemicals associated with nuclear processes (e.g., the reprocessing of uranium to produce plutonium for nuclear weapons, or the separation of actinides from processing waste streams), can provide sticky residues or signatures that will attach to piping, ducting, soil, water, or other surface media. Volatile compounds, that are more suitable for electro-optical sensing, have been well studied. However, the semi-volatile compounds have not been well documented or studied. A majority of these semi-volatile chemicals are more robust than typical gaseous or liquid chemicals and can have lifetimes of several weeks, months, or years in the environment. However, large data gapsmore » exist concerning these potential signature compounds and more research is needed to fill these data gaps so that important signature information is not overlooked or discarded. This report investigates key semi-volatile compounds associated with nuclear separations, identifies available chemical and physical properties, and discusses the degradation products that would result from hydrolysis, radiolysis and oxidation reactions on these compounds.« less

Crystalline Structure and Physical Properties of UCo2Al3

NASA Astrophysics Data System (ADS)

Verdín, E.; Escudero, R.

Some intermetallic compounds which contain uranium or cerium present heavy fermion characteristics. Take, for example, in the UM2Al3 (M=Pd, Ni) family, superconductivity and magnetism coexist and present heavy fermion behavior. This work presents the crystallographic characteristics and physical properties of a new compound of this family; the intermetallic compound UCo2Al3. Our initial crystallographic studies performed in a small single crystal show that the structure is hexagonal and similar to the UNi2Al3 and UPd2Al3 parent compounds. The space group is P6/mmm with a=5.125 Å and c=4.167 Å crystalline parameters. Measurements of resistivity and magnetization performed on the single crystal reveal that the compound is not superconducting when measured at about 1.8 K. The compound is highly anisotropic and features related to Kondo-like behavior are observed. A weak ferromagnetic transition is observed at a temperature of about 20 K.

Measurement of the 235U Induced Fission Gamma-ray Spectrum as an Active Non-destructive Assay of Fresh Nucleear Fuel

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

Sarnoski, Sarah E.; Fast, James E.; Fulsom, Bryan G.

2017-07-17

Non-destructive assay is a powerful tool the International Atomic Energy Agency (IAEA) employs to verify adherence to safeguards agreements. Current IAEA veri- cation techniques for fresh nuclear fuel include passive gamma-ray spectroscopy to determine fuel enrichment. This technique suers from self-shielding and lakes the percision to detect diversion of central fuel rods. The aim of this research is to develop a new, more capable non-destructive analysis technique using active neutron interroga- tion of fuel assemblies and determining the yields of short-lived ssion products from high-resolution gamma-ray spectroscopy using high-purity germanium (HPGe). This paper reports results from irradiation of a onemore » meter tall mock fresh fuel assembly with low enriched uranium (LEU) or depleted uranium (DU) rods using a down-scattered deuterium-tritium (D-T) neutron source. Both prompt and delayed gamma-ray spec- tra were collected as time-stamped list-mode data in a coax detector and without list mode data in a planar strip detector. No dierentiating signatures were observed in the prompt spectra in either detector; however, both detectors observed several short-lived ssion product signatures in LEU and not DU fuel, indicating that this technique has potential for determination of enrichment of fresh fuel assemblies. There were eight unique ssion products observed in the LEU spectra with the coax detector spectra, and three ssion products were observed in the LEU spectra with the strip detector.« less

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Preparative isolation and purification of antioxidative diarylheptanoid derivatives from Alnus japonica by high-speed counter-current chromatography.

PubMed

Lim, Soon Sung; Lee, Min Young; Ahn, Hong Ryul; Choi, Soon Jung; Lee, Jae-Yong; Jung, Sang Hoon

2011-12-01

This study employed the online HPLC-2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS)(+) bioassay to rapidly determine the antioxidant compounds occurring in the crude extract of Alnus japonica. The negative peaks of the ABTS(+) radical scavenging detection system, which indicated the presence of antioxidant activity, were monitored by measuring the decrease in absorbance at 734 nm. The ABTS(+)-based antioxidant activity profile showed that three negative peaks exhibited antioxidant activity. High-speed counter-current chromatography (HSCCC) was used for preparative scale separation of the three active peaks from the extract. The purity of the isolated compounds was analyzed by HPLC and their structures were identified by (1)H- and (13)C-nuclear magnetic resonance spectrometry (NMR), heteronuclear multiple bond correlation (HMBC), and heteronuclear single quantum correlation (HSQC). Two solvent systems composed of n-hexane/ethylacetate/methanol/water (4:6:4:6, v/v) and of ethyl acetate/methanol/water (1:0.1:1, v/v) were performed in high-speed counter-current chromatography. Consequently, a total of 527 mg of hirsutanonol 5-O-β-D-glucopyranoside, 80.04 mg of 3-deoxohirsutenonol 5-O-β-D-glucopyranoside, and 91.0 mg of hirsutenone were obtained with purity of 94.7, 90.5, and 98.6%, respectively. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of programmed-temperature vaporization injection preparative capillary GC for compound specific radiocarbon analysis.

PubMed

Zhang, Xinyu; Zhao, Liang; Wang, Yexin; Xu, Yunping; Zhou, Liping

2013-07-01

Preparative capillary GC (PCGC) is a powerful tool for the separation and purification of compounds from any complex matrix, which can be used for compound-specific radiocarbon analysis. However, the effect of PCGC parameters on the trapping efficiency is not well understood. Here, we present a comprehensive study on the optimization of parameters based on 11 reference compounds with different physicochemical properties. Under the optimum conditions, the trapping efficiencies of these 11 compounds (including high-boiling-point n-hentriacontane and methyl lignocerate) are about 80% (60-89%). The isolation of target compounds from standard solutions, plant and soil samples demonstrates that our optimized method is applicable for different classes of compounds including n-alkanes, fatty acid esters, long-chain fatty alcohol esters, polycyclic aromatic hydrocarbons (PAHs) and steranes. By injecting 25 μL in large volume injection mode, over 100 μg, high purity (>90%) target compounds are harvested within 24 h. The recovery ranges of two real samples are about 70% (59.9-83.8%) and about 83% (77.2-88.5%), respectively. Compared to previous studies, our study makes significant improvement in the recovery of PCGC, which is important for its wide application in biogeochemistry, environmental sciences, and archaeology. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antioxidant, anti-glycation and anti-inflammatory activities of phenolic constituents from Cordia sinensis.

PubMed

Al-Musayeib, Nawal; Perveen, Shagufta; Fatima, Itrat; Nasir, Muhammad; Hussain, Ajaz

2011-12-08

Nine compounds have been isolated from the ethyl acetate soluble fraction of C. sinensis, namely protocatechuic acid (1), trans-caffeic acid (2), methyl rosmarinate (3), rosmarinic acid (4), kaempferide-3-O-β-D-glucopyranoside (5), kaempferol-3-O-β-D-glucopyranoside (6), quercetin-3-O-β-D-glucopyranoside (7), kaempferide-3-O-α-L-rhamnopyranosyl (1→6)-β-D-glucopyranoside (8) and kaempferol-3-O-α-L-rhamno-pyranosyl (1→6)-β-D-glucopyranoside (9), all reported for the first time from this species. The structures of these compounds were deduced on the basis of spectroscopic studies, including 1D and 2D NMR techniques. Compounds 1-9 were investigated for biological activity and showed significant anti-inflammatory activity in the carrageen induced rat paw edema test. The antioxidant activities of isolated compounds 1-9 were evaluated by the DPPH radical scavenging test, and compounds 1, 2, 4 and 7-9 exhibited marked scavenging activity compared to the standard BHA. These compounds were further studied for their anti-glycation properties and some compounds showed significant anti-glycation inhibitory activity. The purity of compounds 2-5, 8 and 9 was confirmed by HPLC. The implications of these results for the chemotaxonomic studies of the genus Cordia have also been discussed.

In situ click chemistry: a powerful means for lead discovery.

PubMed

Sharpless, K Barry; Manetsch, Roman

2006-11-01

Combinatorial chemistry and parallel synthesis are important and regularly applied tools for lead identification and optimisation, although they are often accompanied by challenges related to the efficiency of library synthesis and the purity of the compound library. In the last decade, novel means of lead discovery approaches have been investigated where the biological target is actively involved in the synthesis of its own inhibitory compound. These fragment-based approaches, also termed target-guided synthesis (TGS), show great promise in lead discovery applications by combining the synthesis and screening of libraries of low molecular weight compounds in a single step. Of all the TGS methods, the kinetically controlled variant is the least well known, but it has the potential to emerge as a reliable lead discovery method. The kinetically controlled TGS approach, termed in situ click chemistry, is discussed in this article.

Novel 2-Phenoxyanilide Congeners Derived from a Hit Structure of the TCAMS: Synthesis and Evaluation of Their in Vitro Activity against Plasmodium falciparum.

PubMed

Weidner, Thomas; Nasereddin, Abed; Preu, Lutz; Grünefeld, Johann; Dzikowski, Ron; Kunick, Conrad

2016-02-17

The Tres Cantos Antimalarial Compound Set (TCAMS) is a publicly available compound library which contains 13533 hit structures with confirmed activity against Plasmodium falciparum, the infective agent responsible for malaria tropica. The TCAMS provides a variety of starting points for the investigation of new antiplasmodial drug leads. One of the promising compounds is TCMDC-137332, which seemed to be a good starting point due to its antiplasmodial potency and its predicted physicochemical properties. Several new analogues based on a 2-phenoxyanilide scaffold were synthesized by standard amide coupling reactions and were fully characterized regarding their identity and purity by spectroscopic and chromatographic methods. Furthermore, the results of the biological evaluation of all congeners against Plasmodium falciparum NF54 strains are presented. The findings of our in vitro screening could not confirm the presumed nanomolar antiplasmodial activity of TCMDC-137332 and its derivatives.

Antiplasmodial, beta-haematin inhibition, antitrypanosomal and cytotoxic activity in vitro of novel 4-aminoquinoline 2-imidazolines.

PubMed

Musonda, Chitalu C; Yardley, Vanessa; de Souza, Renata C Carvalho; Ncokazi, Kanyile; Egan, Timothy J; Chibale, Kelly

2008-12-07

A novel series of 4-aminoquinoline-containing 2-imidazolines were synthesized via a one-pot 3-component condensation reaction of amine, aldehyde and isocyanoacetate. The products were obtained in high yield as well as purity and were evaluated directly against two strains of Plasmodium falciparum and Trypanosoma brucei. Compound was the most active across all parasites with ED(50) = 3.3 nM against a chloroquine (CQ)-sensitive 3D7 strain, ED(50) = 33 nM against a CQ-resistant K1 strain and ED(50) = 70 nM against T. brucei. Several compounds were able to inhibit formation of beta-haematin in vitro, suggesting haemozoin formation in the malaria parasite as a possible target. On the other hand, evaluation against a human KB cell line revealed that the compounds were generally non-cytotoxic to the host cells.

Ultra-high vacuum compatible induction-heated rod casting furnace

NASA Astrophysics Data System (ADS)

Bauer, A.; Neubauer, A.; Münzer, W.; Regnat, A.; Benka, G.; Meven, M.; Pedersen, B.; Pfleiderer, C.

2016-06-01

We report the design of a radio-frequency induction-heated rod casting furnace that permits the preparation of polycrystalline ingots of intermetallic compounds under ultra-high vacuum compatible conditions. The central part of the system is a bespoke water-cooled Hukin crucible supporting a casting mold. Depending on the choice of the mold, typical rods have a diameter between 6 mm and 10 mm and a length up to 90 mm, suitable for single-crystal growth by means of float-zoning. The setup is all-metal sealed and may be baked out. We find that the resulting ultra-high vacuum represents an important precondition for processing compounds with high vapor pressures under a high-purity argon atmosphere up to 3 bars. Using the rod casting furnace, we succeeded to prepare large high-quality single crystals of two half-Heusler compounds, namely, the itinerant antiferromagnet CuMnSb and the half-metallic ferromagnet NiMnSb.

Ultra-high vacuum compatible induction-heated rod casting furnace.

PubMed

Bauer, A; Neubauer, A; Münzer, W; Regnat, A; Benka, G; Meven, M; Pedersen, B; Pfleiderer, C

2016-06-01

We report the design of a radio-frequency induction-heated rod casting furnace that permits the preparation of polycrystalline ingots of intermetallic compounds under ultra-high vacuum compatible conditions. The central part of the system is a bespoke water-cooled Hukin crucible supporting a casting mold. Depending on the choice of the mold, typical rods have a diameter between 6 mm and 10 mm and a length up to 90 mm, suitable for single-crystal growth by means of float-zoning. The setup is all-metal sealed and may be baked out. We find that the resulting ultra-high vacuum represents an important precondition for processing compounds with high vapor pressures under a high-purity argon atmosphere up to 3 bars. Using the rod casting furnace, we succeeded to prepare large high-quality single crystals of two half-Heusler compounds, namely, the itinerant antiferromagnet CuMnSb and the half-metallic ferromagnet NiMnSb.

Heavy Fermions

NASA Astrophysics Data System (ADS)

Sugiyama, K.; Ónuki, Y.

Recent experimental results of high-field magnetization and de Haas-van Alphen experiments in f-electron systems are presented. The magnetic moment and the electronic state are simultaneously discussed because both properties are connected with each other. The first example is a drastic change of the Fermi surface in the antiferromagnet NdIn3. The second is the metamagnetic transition based on the quadrupolar interaction in PrCu2. The third is the metamagnetic transition in a typical heavy fermion compound CeRu2Si2, together with the heavy fermion uranium compounds such as UPd2Al3, URu2Si2 and UPt3.

Pressurized liquid extraction coupled with countercurrent chromatography for systematic isolation of chemical constituents by preprogrammed automatic control.

PubMed

Zhang, Yuchi; Guo, Liping; Liu, Chunming; Fu, Zi' ao; Cong, Lei; Qi, Yanjuan; Li, Dongping; Li, Sainan; Wang, Jing

2013-09-15

Pressurized liquid extraction (PLE) coupled with high-speed countercurrent chromatography (HSCCC) via an automated procedure was firstly developed to extract and isolate ginsenosides from Panax quinquefolium. The experiments were designed under the guidance of mathematical model. The partition coefficient (K) values of the target compounds and resolutions of peak profiles were employed as the research indicators, and exponential function and binomial formulas were used to optimizing the solvent systems and flow rates of the mobile phases in a three-stage separation. In the first stage, ethyl acetate, n-butanol, and water were simultaneously pumped into the solvent separator at the flow rates 11.0, 10.0, and 23.0mL/min, respectively. The upper phase of the solvent system in the solvent separator was used as both the PLE solvent and the HSCCC stationary phase, followed by elution with the lower phase of the corresponding solvent system to separate the common ginsenosides. In the second and third stages, rare ginsenosides were first separated by elution with ethyl acetate, n-butanol, methanol, and water (flow rates: 20.0, 3.0, 5.0, and 11.0mL/min, respectively), then with n-heptane, n-butanol, methanol, and water (flow rates: 17.5, 6.0, 5.0, and 22.5mL/min, respectively). Nine target compounds, with purities exceeding 95.0%, and three non-target compounds, with purities above 84.48%, were successfully separated at the semipreparative scale in 450min. The separation results prove that the PLE/HSCCC parameters calculated via mathematical model and formulas were accurately and scientifically. This research has opened up great prospects for industrial automation application. Copyright © 2013 Elsevier B.V. All rights reserved.

Formation of Residual Gases from Source Materials in Closed Crystal Growth Systems

NASA Technical Reports Server (NTRS)

Palosz, W.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Different, non-constituent cases are present in crystal growth systems and may affect processes like growth rate in PVT or voids formation and detached solidification in melt growth systems. The presence of the gas may be detrimental or advantageous depending on its amount and composition, and on the process in question. The presence of the cases, their amount and composition, can be caused and changed by diffusion through and desorption from the growth container material. We have investigated these phenomena for silica glass ampoules. We also found, that residual cases can be generated by the source materials: even very high purity commercial elements and compounds may contain trace amounts of impurities, particularly oxides. The oxides may have low volatilities themselves but their reaction with other species, particularly carbon and hydrogen, may produce volatile compounds like water or carbon oxides. The amount of the gas and its composition is dependent on the original purity of the material (oxide contaminants) and the heat treatment of the source prior to sealing. In many cases. particularly at temperatures below about 900 C and in well-outgassed ampoules, this mechanism dominates. The problem is of a particular importance in sealed systems where the amount and composition of the gas cannot be directly controlled. Therefore, a reasonable knowledge and understanding of the origin, composition, magnitude, and change with time of gases present in sealed ampoules may be important for a meaningful control and interpretation of crystal growth processes. We have investigated this phenomenon in more details for a number of elements and compounds, primarily for II-VI and IV-VI materials. Different source pre-treatment and annealing procedures were applied, and subsequent consecutive annealings and measurements were done to determine the origin and development of the gas in the systems.

Coordination polymer-derived nano-sized zinc ferrite with excellent performance in nitro-explosive detection.

PubMed

Singha, Debal Kanti; Mahata, Partha

2017-08-29

Herein, a mixed metal coordination polymer, {(H 2 pip)[Zn 1/3 Fe 2/3 (pydc-2,5) 2 (H 2 O)]·2H 2 O} 1 {where H 2 pip = piperazinediium and pydc-2,5 = pyridine-2,5-dicarboxylate}, was successfully synthesized using a hydrothermal technique. To confirm the structure and phase purity of 1, single crystals of an isomorphous pure Fe compound, {(H 2 pip)[Fe(pydc-2,5) 2 (H 2 O)]·2H 2 O} 1a, were synthesized based on similar synthetic conditions. Single crystal X-ray data of 1a confirmed the one-dimensional anionic metal-organic coordination polymer hydrogen bonded with protonated piprazine (piperazinediium) and lattice water molecules. The phase purity of 1 and 1a were confirmed via powder X-ray diffraction. Compound 1 was systematically characterized using IR, TGA, SEM, and EDX elemental mapping analysis. Compound 1 was used as a single source precursor for the preparation of nano-sized ZnFe 2 O 4 via thermal decomposition. The as-obtained ZnFe 2 O 4 was fully characterized using PXRD, SEM, TEM, and EDX elemental mapping analysis. It was found that ZnFe 2 O 4 was formed in its pure form with particle size in the nano-dimension. The aqueous dispersion of nano-sized ZnFe 2 O 4 exhibits a strong emission at 402 nm upon excitation at 310 nm. This emissive property was employed for luminescence-based detection of nitroaromatic explosives in an aqueous medium through luminescence quenching for the first time. Importantly, selective detections have been observed for phenolic nitroaromatics based on differential luminescence quenching behaviour along with a detection limit of 57 ppb for 2,4,6-trinitrophenol (TNP) in water.

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.

The biomineralization process of uranium(VI) by Saccharomyces cerevisiae - transformation from amorphous U(VI) to crystalline chernikovite.

PubMed

Shen, Yanghao; Zheng, Xinyan; Wang, Xiaoyu; Wang, Tieshan

2018-05-01

Microorganisms play a significant role in uranium(VI) biogeochemistry and influence U(VI) transformation through biomineralization. In the present work, the process of uranium mineralization was investigated by Saccharomyces cerevisiae. The toxicity experiments showed that the viability of cell was not significantly affected by 100 mg L -1 U(VI) under 4 days of exposure time. The batch experiments showed that the phosphate concentration and pH value increased over time during U(VI) adsorption. Meanwhile, thermodynamic calculations demonstrated that the adsorption system was supersaturated with respect to UO 2 HPO 4 . The X-ray powder diffraction spectroscopy (XRD), field emission scanning electron microscopy (FE-SEM) equipped with energy dispersive spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS) analyses indicated that the U(VI) was first attached onto the cell surface and reacted with hydroxyl, carboxyl, and phosphate groups through electrostatic interactions and complexation. As the immobilization of U(VI) transformed it from the ionic to the amorphous state, lamellar uranium precipitate was formed on the cell surface. With the prolongation of time, the amorphous uranium compound disappeared, and there were some crystalline substances observed extracellularly, which were well-characterized as tetragonal-chernikovite. Furthermore, the size of chernikovite was regulated at nano-level by cells, and the perfect crystal was formed finally. These findings provided an understanding of the non-reductive transformation process of U(VI) from the amorphous to crystalline state within microbe systems, which would be beneficial for the U(VI) treatment and reuse of nuclides and heavy metals.

Desferrithiocin Analogue Uranium Decorporation Agents

PubMed Central

Bergeron, Raymond J.; Wiegand, Jan; Singh, Shailendra

2010-01-01

Purpose Previous systematic structure-activity studies of the desferrithiocin (DFT) platform have allowed the design and synthesis of analogues and derivatives of DFT that retain the exceptional iron-clearing activity of the parent, while eliminating its adverse effects. We hypothesized that a similar approach could be adopted to identify DFT-related analogues that could effectively decorporate uranium. Materials and Methods The decorporation properties of nine DFT-related analogues were determined in a bile duct-cannulated rat model. Diethylenetriaminepentaacetic acid (DTPA) served as a positive control. Selected ligands also underwent multiple and delayed dosing regimens. Uranium excretion in urine and bile or stool was determined by inductively coupled plasma mass spectroscopy (ICP-MS); tissue levels of uranium were also assessed. Results The two best clinical candidates are (S)-4,5-dihydro-2-[2-hydroxy-4-(3,6,9-trioxadecyloxy)phenyl]-4-methyl-4-thiazolecarboxylic acid [(S)-4'-(HO)-DADFT-PE (9)], with a 57% reduction in kidney uranium levels on oral (p.o.) administration and (S)-4,5-dihydro-2-[2-hydroxy-3-(3,6,9-trioxadecyloxy)phenyl]-4-methyl-4-thiazolecarboxylic acid [(S)-3'-(HO)-DADFT-PE (10)], with a 62% renal reduction on p.o. administration. The majority of the metal excretion promoted by these analogues is in the bile, thus further reducing kidney actinide exposure. Conclusions While 9 administered p.o. or subcutaneously (s.c.) immediately post-metal is an effective decorporation agent, withholding the dose (s.c.) until 4 h reduced the activity of the compound. Conversion of 9 to its isopropyl ester may circumvent this issue. PMID:19399680

First-principles study of uranium carbide: Accommodation of point defects and of helium, xenon, and oxygen impurities

NASA Astrophysics Data System (ADS)

Freyss, Michel

2010-01-01

Point defects and volatile impurities (helium, xenon, oxygen) in uranium monocarbide UC are studied by first-principles calculations. Preliminarily, bulk properties of UC and of two other uranium carbide phases, UC2 and U2C3 , are calculated in order to compare them to experimental data and to get confidence in the use of the generalized gradient approximation for this class of compounds. The subsequent study of different types of point defects shows that the carbon sublattice best accommodates the defects. The perturbation of the crystal structure induced by the defects is weak and the interaction between defects is found short range. Interstitial carbon dumbbells possibly play an important role in the diffusion of carbon atoms. The most favorable location of diluted helium, xenon, and oxygen impurities in the UC crystal lattice is then determined. The rare-gas atoms occupy preferably a uranium substitution site or a uranium site in a U-C bivacancy. But their incorporation in UC is, however, not energetically favorable, especially for xenon, suggesting their propensity to diffuse in the material and/or form bubbles. On the other hand, oxygen atoms are very favorably incorporated as diluted atoms in the UC lattice, confirming the easy oxidation of UC. The oxygen atoms preferably occupy a carbon substitution site or the carbon site of a U-C bivacancy. Our results are compared to available experimental data on UC and to similar studies by first-principles calculations for other carbides and nitrides with the rock-salt structure.

Argon/UF6 plasma experiments: UF6 regeneration and product analysis

NASA Technical Reports Server (NTRS)

Roman, W. C.

1980-01-01

An experimental and analytical investigation was conducted to aid in developing some of the technology necessary for designing a self-critical fissioning uranium plasma core reactors (PCR). This technology is applicable to gaseous uranium hexafluoride nuclear-pumped laser systems. The principal equipment used included 1.2 MW RF induction heater, a d.c. plasma torch, a uranium tetrafluoride feeder system, and batch-type fluorine/UF6 regeneration systems. Overall objectives were to continue to develop and test materials and handling techniques suitable for use with high-temperature, high-pressure, gaseous UF6; and to continue development of complementary diagnostic instrumentation and measurement techniques to characterize the effluent exhaust gases and residue deposited on the test chamber and exhaust system components. Specific objectives include: a development of a batch-type UF6 regeneration system employing pure high-temperature fluorine; development of a ruggedized time-of-flight mass spectrometer and associated data acquisition system capable of making on-line concentration measurements of the volatile effluent exhaust gas species in a high RF environment and corrosive environment of UF6 and related halide compounds.

Quantitative ion beam analysis of M-C-O systems: application to an oxidized uranium carbide sample

NASA Astrophysics Data System (ADS)

Martin, G.; Raveu, G.; Garcia, P.; Carlot, G.; Khodja, H.; Vickridge, I.; Barthe, M. F.; Sauvage, T.

2014-04-01

A large variety of materials contain both carbon and oxygen atoms, in particular oxidized carbides, carbon alloys (as ZrC, UC, steels, etc.), and oxycarbide compounds (SiCO glasses, TiCO, etc.). Here a new ion beam analysis methodology is described which enables quantification of elemental composition and oxygen concentration profile over a few microns. It is based on two procedures. The first, relative to the experimental configuration relies on a specific detection setup which is original in that it enables the separation of the carbon and oxygen NRA signals. The second concerns the data analysis procedure i.e. the method for deriving the elemental composition from the particle energy spectrum. It is a generic algorithm and is here successfully applied to characterize an oxidized uranium carbide sample, developed as a potential fuel for generation IV nuclear reactors. Furthermore, a micro-beam was used to simultaneously determine the local elemental composition and oxygen concentration profiles over the first microns below the sample surface. This method is adapted to the determination of the composition of M?C?O? compounds with a sensitivity on elemental atomic concentrations around 1000 ppm.

CONTINUOUS PROCESS FOR PREPARING URANIUM HEXAFLUORIDE FROM URANIUM TETRAFLUORIDE AND OXYGEN

DOEpatents

Adams, J.B.; Bresee, J.C.; Ferris, L.M.

1961-11-21

A process for preparing UF/sub 6/ by reacting UF/sub 4/ and oxygen is described. The UF/sub 4/ and oxygen are continuously introduced into a fluidized bed of UO/sub 2/F/sub 2/ at a temperature of 600 to 900 deg C. The concentration of UF/sub 4/ in the bed is maintained below 25 weight per cent in order to avoid sintering and intermediate compound formation. By-product U0/sub 2/F/sub 2/ is continuously removed from the top of the bed recycled. In an alternative embodiment heat is supplied to the reaction bed by burning carbon monoxide in the bed. The product UF/sub 6/ is filtered to remove entrained particles and is recovered in cold traps and chemical traps. (AEC)

Surface spectroscopy studies of the oxidation behavior of uranium

NASA Astrophysics Data System (ADS)

Bloch, J.; Atzmony, U.; Dariel, M. P.; Mintz, M. H.; Shamir, N.

1982-02-01

Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) techniques were utilized to study the oxidation behavior of clean uranium surfaces, at very low pressures of various atmospheres (UHV, H 2, O 2, and CO 2), at room temperature. Both for O 2 and CO 2, a precursor chemisorbed oxygen species has been identified at the very initial stage of the oxidation reaction. This chemisorbed oxygen transforms to the oxide form at a rate which depends on the pressure of the oxidizing atmosphere. Residual gaseous carbon compounds which are present even under UHV conditions result in the simultaneous formation of surface carbide which accompanies the initial stage of oxidation. This carbide however decomposes later as oxidation proceeds. Adventitious hydrocarbon adsorption occurs on the formed oxide layer.

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

PubMed

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

2018-02-15

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

Purification and Crystal Growth of Lead Iodide by Physical Vapor Transport Method

NASA Technical Reports Server (NTRS)

Wright, G. W.; Cole, M.; Chen, Y.-F.; Chen, K.-T.; Chen, H.; Chattopadhyay, K.; Burger, A.

1998-01-01

Lead iodide (PbI2) is a layered compound semiconductor being developed as room temperature x- and gamma-ray detector. Compared to the more studied material, mercuric iodide, PbI2 has a higher melting temperature and no phase transition until liquid phase which are indications of better mechanical properties. In this study, the source material was purified by the zone-refining process, and the purest section was extracted from center of the the zone-refined ingot to be grown by physical vapor transport (PVT) method. The zone-refined material and as-grown crystals were characterized by optical microscopy and differential scanning calorimetry (DSC) to reveal the surface morphology, purity and stoichiometry. The results shows that both materials are near-stoichiometric composition, with the purity of the as-grown crystals higher than zone-refined materials. The resistivity of the as-grown crystal (10" Omega-cm) was derived from current-voltage (I-V) measurement, and is 10 times higher than the zone-refined materials. Detail results will be presented and discussed.

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

PubMed

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

2011-09-01

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

Isoflavones in food supplements: chemical profile, label accordance and permeability study in Caco-2 cells.

PubMed

Almeida, I M C; Rodrigues, F; Sarmento, B; Alves, R C; Oliveira, M B P P

2015-03-01

Consumers nowadays are playing an active role in their health-care. A special case is the increasing number of women, who are reluctant to use exogenous hormone therapy for the treatment of menopausal symptoms and are looking for complementary therapies. However, food supplements are not clearly regulated in Europe. The EFSA has only recently begun to address the issues of botanical safety and purity regulation, leading to a variability of content, standardization, dosage, and purity of available products. In this study, isoflavones (puerarin, daidzin, genistin, daidzein, glycitein, genistein, formononetin, prunetin, and biochanin A) from food supplements (n = 15) for menopausal symptoms relief are evaluated and compared with the labelled information. Only four supplements complied with the recommendations made by the EC on the tolerable thresholds. The intestinal bioavailability of these compounds was investigated using Caco-2 cells. The apparent permeability coefficients of the selected isoflavonoids across the Caco-2 cells were affected by the isoflavone concentration and product matrix.

Ground-Water Quality of the Northern High Plains Aquifer, 1997, 2002-04

USGS Publications Warehouse

Stanton, Jennifer S.; Qi, Sharon L.

2007-01-01

An assessment of ground-water quality in the northern High Plains aquifer was completed during 1997 and 2002-04. Ground-water samples were collected at 192 low-capacity, primarily domestic wells in four major hydrogeologic units of the northern High Plains aquifer-Ogallala Formation, Eastern Nebraska, Sand Hills, and Platte River Valley. Each well was sampled once, and water samples were analyzed for physical properties and concentrations of nitrogen and phosphorus compounds, pesticides and pesticide degradates, dissolved solids, major ions, trace elements, dissolved organic carbon (DOC), radon, and volatile organic compounds (VOCs). Tritium and microbiology were analyzed at selected sites. The results of this assessment were used to determine the current water-quality conditions in this subregion of the High Plains aquifer and to relate ground-water quality to natural and human factors affecting water quality. Water-quality analyses indicated that water samples rarely exceeded established U.S. Environmental Protection Agency public drinking-water standards for those constituents sampled; 13 of the constituents measured or analyzed exceeded their respective standards in at least one sample. The constituents that most often failed to meet drinking-water standards were dissolved solids (13 percent of samples exceeded the U.S. Environmental Protection Agency Secondary Drinking-Water Regulation) and arsenic (8 percent of samples exceeded the U.S. Environmental Protection Agency Maximum Contaminant Level). Nitrate, uranium, iron, and manganese concentrations were larger than drinking-water standards in 6 percent of the samples. Ground-water chemistry varied among hydrogeologic units. Wells sampled in the Platte River Valley and Eastern Nebraska units exceeded water-quality standards more often than the Ogallala Formation and Sand Hills units. Thirty-one percent of the samples collected in the Platte River Valley unit had nitrate concentrations greater than the standard, 22 percent exceeded the manganese standard, 19 percent exceeded the sulfate standard, 26 percent exceeded the uranium standard, and 38 percent exceeded the dissolved-solids standard. In addition, 78 percent of samples had at least one detectable pesticide and 22 percent of samples had at least one detectable VOC. In the Eastern Nebraska unit, 30 percent of the samples collected had dissolved-solids concentrations larger than the standard, 23 percent exceeded the iron standard, 13 percent exceeded the manganese standard, 10 percent exceeded the arsenic standard, 7 percent exceeded the sulfate standard, 7 percent exceeded the uranium standard, and 7 percent exceeded the selenium standard. No samples exceeded the nitrate standard. Thirty percent of samples had at least one detectable pesticide compound and 10 percent of samples had at least one detectable VOC. In contrast, the Sand Hills and Ogallala Formation units had fewer detections of anthropogenic compounds and drinking-water exceedances. In the Sand Hills unit, 15 percent of the samples exceeded the arsenic standard, 4 percent exceeded the nitrate standard, 4 percent exceeded the uranium standard, 4 percent exceeded the iron standard, and 4 percent exceeded the dissolved-solids standard. Fifteen percent of samples had at least one pesticide compound detected and 4 percent had at least one VOC detected. In the Ogallala Formation unit, 6 percent of water samples exceeded the arsenic standard, 4 percent exceeded the dissolved-solids standard, 3 percent exceeded the nitrate standard, 2 percent exceeded the manganese standard, 1 percent exceeded the iron standard, 1 percent exceeded the sulfate standard, and 1 percent exceeded the uranium standard. Eight percent of samples collected in the Ogallala Formation unit had at least one pesticide detected and 6 percent had at least one VOC detected. Differences in ground-water chemistry among the hydrogeologic units were attributed to variable depth to water, depth of the well screen below the water table, reduction-oxidation conditions, ground-water residence time, interactions with surface water, composition of aquifer sediments, extent of cropland, extent of irrigated land, and fertilizer application rates.

Consequences of electroplated targets on radiopharmaceutical preparations

NASA Astrophysics Data System (ADS)

Finn, R. D.; Tirelli, S.; Sheh, Y.; Knott, A.; Gelbard, A. S.; Larson, S. M.; Dahl, J. R.

1991-05-01

The staff of the cyclotron facility at Memorial Sloan-Kettering Cancer Center is involved in a comprehensive radionuclide preparation program which culminates with the formulation of numerous requested short-lived, positron-emitting radiopharmaceutical agents for clinical investigation. Both the produced radionuclide as well as the final radiolabeled compound are subjected to stringent quality control standards including assays for radiochemical and chemical purity. The subtle chemical consequences resulting from the irradiation of a nickel-plated target for 13N production serve to emphasize some of these potential technical difficulties.

Synthesis of Enantiomerically Pure 6-Substituted-Piperazine-2-Acetic Acid Esters as Intermediates for Library Production.

PubMed

Chamakuri, Srinivas; Jain, Prashi; Guduru, Shiva Krishna Reddy; Arney, Joseph Winston; MacKenzie, Kevin; Santini, Conrad; Young, Damian W

2018-05-11

Amino acids from the chiral pool have been used to produce a 24-member branch of 2,6-disubstituted piperazine scaffolds suitable for use in compound library production. Each scaffold was obtained as a single absolute stereoisomer in multi-gram quantities. Stereochemistry was confirmed by 2D NMR protocols and enantiomeric purity was determined by chiral HPLC. The scaffolds are intended for use as intermediates in parallel synthesis of small-molecule libraries.

Csbnd N bond formation in alicyclic and heterocyclic compounds by amine-modified nanoclay

NASA Astrophysics Data System (ADS)

Zarnegar, Zohre; Alizadeh, Roghayeh; Ahmadzadeh, Majid; Safari, Javad

2017-09-01

In the current protocol, amine functionalized montmorillonite K10 nanoclay (NH2-MMT) was applied to catalyze the formation of Csbnd N bonds in the synthesis of azines and 2-aminothiazoles at room temperature. In comparison with the current methods of Csbnd N bond formation, this approach displays specific advantages include atom economy, clean conversion, design for energy efficiency, the use of nontoxic and heterogeneous catalyst, higher purity and yields, safer solvent and reagents for this organic transformation.

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

PubMed Central

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

2015-01-01

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

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

PubMed

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

2015-02-06

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

Measures of the environmental footprint of the front end of the nuclear fuel cycle

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

E. Schneider; B. Carlsen; E. Tavrides

2013-11-01

Previous estimates of environmental impacts associated with the front end of the nuclear fuel cycle (FEFC) have focused primarily on energy consumption and CO2 emissions. Results have varied widely. This work builds upon reports from operating facilities and other primary data sources to build a database of front end environmental impacts. This work also addresses land transformation and water withdrawals associated with the processes of the FEFC. These processes include uranium extraction, conversion, enrichment, fuel fabrication, depleted uranium disposition, and transportation. To allow summing the impacts across processes, all impacts were normalized per tonne of natural uranium mined as wellmore » as per MWh(e) of electricity produced, a more conventional unit for measuring environmental impacts that facilitates comparison with other studies. This conversion was based on mass balances and process efficiencies associated with the current once-through LWR fuel cycle. Total energy input is calculated at 8.7 x 10- 3 GJ(e)/MWh(e) of electricity and 5.9 x 10- 3 GJ(t)/MWh(e) of thermal energy. It is dominated by the energy required for uranium extraction, conversion to fluoride compound for subsequent enrichment, and enrichment. An estimate of the carbon footprint is made from the direct energy consumption at 1.7 kg CO2/MWh(e). Water use is likewise dominated by requirements of uranium extraction, totaling 154 L/MWh(e). Land use is calculated at 8 x 10- 3 m2/MWh(e), over 90% of which is due to uranium extraction. Quantified impacts are limited to those resulting from activities performed within the FEFC process facilities (i.e. within the plant gates). Energy embodied in material inputs such as process chemicals and fuel cladding is identified but not explicitly quantified in this study. Inclusion of indirect energy associated with embodied energy as well as construction and decommissioning of facilities could increase the FEFC energy intensity estimate by a factor of up to 2.« less

Highly Sensitive and Selective Uranium Detection in Natural Water Systems Using a Luminescent Mesoporous Metal-Organic Framework Equipped with Abundant Lewis Basic Sites: A Combined Batch, X-ray Absorption Spectroscopy, and First Principles Simulation Investigation.

PubMed

Liu, Wei; Dai, Xing; Bai, Zhuanling; Wang, Yanlong; Yang, Zaixing; Zhang, Linjuan; Xu, Lin; Chen, Lanhua; Li, Yuxiang; Gui, Daxiang; Diwu, Juan; Wang, Jianqiang; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao

2017-04-04

Uranium is not only a strategic resource for the nuclear industry but also a global contaminant with high toxicity. Although several strategies have been established for detecting uranyl ions in water, searching for new uranium sensor material with great sensitivity, selectivity, and stability remains a challenge. We introduce here a hydrolytically stable mesoporous terbium(III)-based MOF material compound 1, whose channels are as large as 27 Å × 23 Å and are equipped with abundant exposed Lewis basic sites, the luminescence intensity of which can be efficiently and selectively quenched by uranyl ions. The detection limit in deionized water reaches 0.9 μg/L, far below the maximum contamination standard of 30 μg/L in drinking water defined by the United States Environmental Protection Agency, making compound 1 currently the only MOF material that can achieve this goal. More importantly, this material exhibits great capability in detecting uranyl ions in natural water systems such as lake water and seawater with pH being adjusted to 4, where huge excesses of competing ions are present. The uranyl detection limits in Dushu Lake water and in seawater were calculated to be 14.0 and 3.5 μg/L, respectively. This great detection capability originates from the selective binding of uranyl ions onto the Lewis basic sites of the MOF material, as demonstrated by synchrotron radiation extended X-ray adsorption fine structure, X-ray adsorption near edge structure, and first principles calculations, further leading to an effective energy transfer between the uranyl ions and the MOF skeleton.

Draft Genome Sequence of Pedobacter sp. Strain NL19, a Producer of Potent Antibacterial Compounds

PubMed Central

2015-01-01

Here, we report the draft genome sequence of Pedobacter sp. strain NL19. The genome has 5.99 Mbp and a G+C content of 39.0%. NL19 was isolated from sludge from an abandoned uranium mine in the north of Portugal, and it produces potent antibacterials against Gram-positive and Gram-negative bacteria. PMID:25814603

Radiolytic Effects on Fluoride Impurities in a U{sub 3}O{sub 8} Matrix

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

Icenhour, A.S.

2000-05-01

The safe handling and storage of radioactive materials require an understanding of the effects of radiolysis on those materials. Radiolysis may result in the production of gases (e.g., corrosives) or pressures that are deleterious to storage containers. A study has been performed to address these concerns as they relate to the radiolysis of residual fluoride compounds in uranium oxides.

Hydrothermal Testing of K Basin Sludge and N Reactor Fuel at Sludge Treatment Project Operating Conditions

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

Delegard, Calvin H.; Schmidt, Andrew J.; Thornton, Brenda M.

The Sludge Treatment Project (STP), managed for the U. S. DOE by Fluor Hanford (FH), was created to design and operate a process to eliminate uranium metal from K Basin sludge prior to packaging for Waste Isolation Pilot Plant (WIPP). The STP process uses high temperature liquid water to accelerate the reaction, produce uranium dioxide from the uranium metal, and safely discharge the hydrogen. Under nominal process conditions, the sludge will be heated in pressurized water at 185°C for as long as 72 hours to assure the complete reaction (corrosion) of up to 0.25-inch diameter uranium metal pieces. Under contractmore » to FH, the Pacific Northwest National Laboratory (PNNL) conducted bench-scale testing of the STP hydrothermal process in November and December 2006. Five tests (~50 ml each) were conducted in sealed, un-agitated reaction vessels under the hydrothermal conditions (e.g., 7 to 72 h at 185°C) of the STP corrosion process using radioactive sludge samples collected from the K East Basin and particles/coupons of N Reactor fuel also taken from the K Basins. The tests were designed to evaluate and understand the chemical changes that may be occurring and the effects that any changes would have on sludge rheological properties. The tests were not designed to evaluate engineering aspects of the process. The hydrothermal treatment affected the chemical and physical properties of the sludge. In each test, significant uranium compound phase changes were identified, resulting from dehydration and chemical reduction reactions. Physical properties of the sludge were significantly altered from their initial, as-settled sludge values, including, shear strength, settled density, weight percent water, and gas retention.« less

Background radiation and individual dosimetry in the costal area of Tamil Nadu, India.

PubMed

Matsuda, Naoki; Brahmanandhan, G M; Yoshida, Masahiro; Takamura, Noboru; Suyama, Akihiko; Koguchi, Yasuhiro; Juto, Norimichi; Raj, Y Lenin; Winsley, Godwin; Selvasekarapandian, S

2011-07-01

South coast of India is known as the high-level background radiation area (HBRA) mainly due to beach sands that contain natural radionuclides as components of the mineral monazite. The rich deposit of monazite is unevenly distributed along the coastal belt of Tamil Nadu and Kerala. An HBRA site that laid in 2×7 m along the sea was found in the beach of Chinnavillai, Tamil Nadu, where the maximum ambient dose equivalent reached as high as 162.7 mSv y(-1). From the sands collected at the HBRA spot, the high-purity germanium semi-conductor detector identified six nuclides of thorium series, four nuclides of uranium series and two nuclides belonging to actinium series. The highest radioactivity observed was 43.7 Bq g(-1) of Th-228. The individual dose of five inhabitants in Chinnavillai, as measured by the radiophotoluminescence glass dosimetry system, demonstrated the average dose of 7.17 mSv y(-1) ranging from 2.79 to 14.17 mSv y(-1).

Detection of pulsed bremsstrahlung-induced prompt neutron capture gamma rays with a HPGe detector

NASA Astrophysics Data System (ADS)

Jones, James L.

1997-02-01

The Idaho National Engineering Laboratory (INEL) is developing a novel photoneutron-based nondestructive evaluation technique which uses a pulsed, high-energy electron accelerator and gamma-ray spectrometry. Highly penetrating pulses of bremsstrahlung photons are produced by each pulse of electrons. Interrogating neutrons are generated by the bremsstrahlung photons interacting within a photoneutron source material. The interactions of the neutrons within a target result in the emission of elemental characteristic gamma-rays. Spectrometry is performed by analyzing the photoneutron-induced, prompt gama-rays acquired between accelerator pulses with a unique, high- purity germanium gamma-ray detection system using a modified transistor reset preamplifier. The detection system, the experimental configuration, and the accelerator operation used to characterize the detection systems performance are described. Using a 6.5-MeV electron accelerator and a beryllium metal photoneutron source, gamma-ray spectra were successfully acquired for Al, Cu, polyethylene, NaCl, and depleted uranium targets as soon as 30 microsecond(s) after each bremsstrahlung flash.

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

Voorhees, D.R.

The Tritium Storage and Delivery System (TSDS) at TFTR was fabricated at Monsanto Mound Lab in the late 1970`s and delivered to PPPL in the early 1980`s. Commissioning progressed slowly and was finally completed in 1992 following a series of Preoperational tests and Integrated Systems tests. Those tests included thorough leak testing of glove boxes and process piping, electrical interlocks and controls, instrumentation calibrations, volume determinations and verification of uranium bed capacity. The system accepted tritium in dilute form in May of 1993 and began serious usage of pure tritium in November 1993. As the throughput of high purity tritiummore » increased, shortcomings of the system became evident and extensive repairs were implemented. System leakage and material compatibility were the primary causes of the problems. To date, the system has received, stored and delivered over 500 kCi of tritium and is performing very well. The dedicated quadrupole mass spectrometer and beta scintillator system has been analyzing tritium bearing and pure gas streams for over 3 years with minimal downtime.« less

Nondestructive Analysis of MET-5 Paint Can at TA35 Building 2 A-Wing Vault

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

Desimone, David J.; Vo, Duc Ta

In Building 2 A-wing vault MET-5 has some drums and other packages they wanted NEN-1 help identifying nondestructively. Measurements using a mechanically cooled portable high-purity germanium HPGe Ortec detective were taken of a paint can container labeled DU-2A to determine if any radioactive material was inside. The HPGe detector measures the gamma rays emitted by radioactive material and displays it as a spectrum. The spectrum is used to identify this radioactive material by using appropriate analysis software and identifying the gamma ray peaks. A paint can container, DU-2A, was analyzed with PeakEasy 4.84 and FRAM 5.2. The FRAM report ismore » shown. The enrichment is 0.091% U235 and 99.907% U238. This material is depleted uranium. The measurement was performed in the near field, and to extract a mass a far field measurement will need to be taken.« less

Recovery of Li from alloys of Al- Li and Li- Al using engineered scavenger compounds

DOEpatents

Riley, W. D.; Jong, B. W.; Collins, W. K.; Gerdemann, S. J.

1994-01-01

A method of producing lithium of high purity from lithium aluminum alloys using an engineered scavenger compound, comprising: I) preparing an engineered scavenger compound by: a) mixing and heating compounds of TiO2 and Li2CO3 at a temperature sufficient to dry the compounds and convert Li.sub.2 CO.sub.3 to Li.sub.2 O; and b) mixing and heating the compounds at a temperature sufficient to produce a scavenger Li.sub.2 O.3TiO.sub.2 compound; II) loading the scavenger into one of two electrode baskets in a three electrode cell reactor and placing an Al-Li alloy in a second electrode basket of the three electrode cell reactor; III) heating the cell to a temperature sufficient to enable a mixture of KCl-LiCl contained in a crucible in the cell to reach its melting point and become a molten bath; IV) immersing the baskets in the bath until an electrical connection is made between the baskets to charge the scavenger compound with Li until there is an initial current and voltage followed by a fall off ending current and voltage; and V) making a connection between the basket electrode containing engineered scavenger compound and a steel rod electrode disposed between the basket electrodes and applying a current to cause Li to leave the scavenger compound and become electrodeposited on the steel rod electrode.

Sulfur-Modified Zero-Valent Iron for Remediation Applications at DOE Sites - 13600

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

Fogwell, Thomas W.; Santina, Pete

2013-07-01

Many DOE remediation sites have chemicals of concern that are compounds in higher oxidation states, which make them both more mobile and more toxic. The chemical reduction of these compounds both prevents the migration of these chemicals and in some cases reduces the toxicity. It has also been shown that zero-valent iron is a very effective substance to use in reducing oxygenated compounds in various treatment processes. These have included the treatment of halogenated hydrocarbons in the form volatile organic compounds used as solvents and pesticides. Zero-valent iron has also been used to reduce various oxidized metals such as chromium,more » arsenic, and mercury in order to immobilize them, decrease their toxicity, and prevent further transport. In addition, it has been used to immobilize or break down other non-metallic species such as selenium compounds and nitrates. Of particular interest at several DOE remediation sites is the fact that zero-valent iron is very effective in immobilizing several radioactive metals which are mobile in their oxidized states. These include both technetium and uranium. The main difficulty in using zero-valent iron has been its tendency to become inactive after relatively short periods of time. While it is advantageous to have the zero-valent iron particles as porous as possible in order to provide maximum surface area for reactions to take place, these pores can become clogged when the iron is oxidized. This is due to the fact that ferric oxide has a greater volume for a given mass than metallic iron. When the surfaces of the iron particles oxidize to ferric oxide, the pores become narrower and will eventually shut. In order to minimize the degradation of the chemical activity of the iron due to this process, a modification of zero-valent iron has been developed which prevents or slows this process, which decreases its effectiveness. It is called sulfur-modified iron, and it has been produced in high purity for applications in municipal water treatment applications. Sulfur-modified iron has been found to not only be an extremely economical treatment technology for municipal water supplies, where very large quantities of water must be treated economically, but it has also been demonstrated to immobilize technetium. It has the added benefit of eliminating several other harmful chemicals in water supplies. These include arsenic and selenium. In one large-scale evaluation study an integrated system implemented chemical reduction of nitrate with sulfur-modified iron followed by filtration for arsenic removal. The sulfur-modified iron that was used was an iron-based granular medium that has been commercially developed for the removal of nitrate, co-contaminants including uranium, vanadium and chromium, and other compounds from water. The independent study concluded that 'It is foreseen that the greatest benefit of this technology (sulfur-modified iron) is that it does not produce a costly brine stream as do the currently accepted nitrate removal technologies of ion exchange and reverse osmosis. This investigation confirmed that nitrate reduction via sulfur-modified iron is independent of the hydraulic loading rate. Future sulfur-modified iron treatment systems can be designed without restriction of the reactor vessel dimensions. Future vessels can be adapted to existing site constraints without being limited to height-to-width ratios that would exist if nitrate reduction were to depend on hydraulic loading rate'. Sulfur-modified iron was studied by the Pacific Northwest National Laboratory (PNNL) for its effectiveness in the reduction and permanent sequestration of technetium. The testing was done using Hanford Site groundwater together with sediment. The report stated, 'Under reducing conditions, TcO{sub 4} is readily reduced to TcIV, which forms highly insoluble oxides such at TcO{sub 2}.nH{sub 2}O. However, (re)oxidation of TcIV oxides can lead to remobilization. Under sulfidogenic conditions, most TcIV will be reduced and immobilized as Tc{sub 2}S{sub 7}, which is less readily re-mobilized, even under oxic conditions. This process should be favored by stimulation of sulfidogenic conditions'. The sulfur-modified iron provides the sulfur, together with the iron, to maintain this stable sequestration of technetium. As a result of these and other studies demonstrating the cost-effectiveness of sulfur-modified iron in treating technetium and other hazardous compounds in Hanford Site groundwater and its cost-effectiveness in reducing nitrate, the Richland Operations Office of the Department of Energy issued a change order to the Central Plateau Contractor providing for the testing of sulfur-modified iron in a mobile pilot unit at the Hanford Site. Further testing is anticipated to produce refinements in operating conditions and further optimization of the existing process. (authors)« less

Preparative isolation and purification of senkyunolide-I, senkyunolide-H and ferulic acid from Rhizoma Chuanxiong using counter-current chromatography.

PubMed

Wei, Yun; Hu, Jia; Li, Hao; Liu, Jiangang

2011-12-01

Three active compounds, senkyunolide-I, senkyunolide-H and ferulic acid (FA), were successfully isolated and purified from the extracts of Rhizoma Chuanxiong by counter-current chromatography (CCC). Based on the principle of the partition coefficient values (k) for target compounds and the separation factor (α) between target compounds, the two-phase solvent system that contains n-hexane-ethyl acetate-methanol-water at an optimized volume ratio of 3:7:4:6 v/v was selected for the CCC separation, and the lower phase was employed as the mobile phase in the head-to-tail elution mode. In a single run, 400 mg of the crude extract yielded pure senkyunolide-I (6.4 mg), senkyunolide-H (1.7 mg) and FA (4.4 mg) with the purities of 98, 93 and 99%, respectively. The CCC fractions were analyzed by high-performance liquid chromatography, and the structures of the three active compounds were identified by MS and (1)H NMR. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Search for Compounds with Hypoglycemic Activity in the Series of 1-[2-(1H-Tetrazol-5-yl)-R1-phenyl]-3-R2-phenyl(ethyl)ureas and R1-Tetrazolo[1,5-c]quinazolin-5(6H)-ones

PubMed Central

Antypenko, Oleksii M.; Kovalenko, Sergiy I.; Zhernova, Galina O.

2016-01-01

Methods of 1-[2-(1H-tetrazol-5-yl)-R1-phenyl]-3-R2-phenyl(ethyl)ureas and R1-tetrazolo[1,5-c]quinazolin-5(6H)-ones synthesis were designed. IR, LC-MS, 1H NMR, and elemental analysis data evaluated the structure and purity of the obtained compounds. Different products, depending on the reaction conditions, were distinguished and discussed. The preliminary hypoglycemic activity of 36 synthesized compounds was revealed. Docking studies to 11β-hydroxysteroid dehydrogenase 1, γ-peroxisome proliferator-activated receptor, and dipeptidyl peptidase-4 were conducted. Eight of these substances were further tested on glucocorticoid-induced insulin resistance models, namely glucose tolerance, oral rapid insulin, and adrenalin tests. One of the most active compounds turned out to be tetrazolo[1,5-c]quinazolin-5(6H)-one 3.1, exceeding the reference drugs Metformin (50 and 200 mg/kg) and Gliclazide (50 mg/kg). PMID:27222601

Universal, In Situ Transformation of Bulky Compounds into Nanoscale Catalysts by High-Temperature Pulse.

PubMed

Xu, Shaomao; Chen, Yanan; Li, Yiju; Lu, Aijiang; Yao, Yonggang; Dai, Jiaqi; Wang, Yanbin; Liu, Boyang; Lacey, Steven D; Pastel, Glenn R; Kuang, Yudi; Danner, Valencia A; Jiang, Feng; Fu, Kun Kelvin; Hu, Liangbing

2017-09-13

The synthesis of nanoscale metal compound catalysts has attracted much research attention in the past decade. The challenges of preparation of the metal compound include the complexity of the synthesis process and difficulty of precise control of the reaction conditions. Herein, we report an in situ synthesis of nanoparticles via a high-temperature pulse method where the bulk material acts as the precursor. During the process of rapid heating and cooling, swift melting, anchoring, and recrystallization occur, resulting in the generation of high-purity nanoparticles. In our work, the cobalt boride (Co 2 B) nanoparticles with a diameter of 10-20 nm uniformly anchored on the reduced graphene oxide (rGO) nanosheets were successfully prepared using the high temperature pulse method. The as-prepared Co 2 B/rGO composite displayed remarkable electrocatalytic performance for the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER). We also prepared molybdenum disulfide (MoS 2 ) and cobalt oxide (Co 3 O 4 ) nanoparticles, thereby demonstrating that the high-temperature pulse is a universal method to synthesize ultrafine metal compound nanoparticles.

[Rapid determination of volatile organic compounds in workplace air by protable gas chromatography-mass spectrometer].

PubMed

Zhu, H B; Su, C J; Tang, H F; Ruan, Z; Liu, D H; Wang, H; Qian, Y L

2017-10-20

Objective: To establish a method for rapid determination of 47 volatile organic compounds in the air of workplace using portable gas chromatography - mass spectrometer(GC - MS). Methods: The mixed standard gas with different concentration levels was made by using the static gas distribution method with the high purity nitrogen as dilution gas. The samples were injected into the GC - MS by a hand - held probe. Retention time and characteristic ion were used for qualitative analysis,and the internal standard method was usd for quantitation. Results: The 47 poisonous substances were separated and determined well. The linear range of this method was 0.2 - 16.0 mg/m(3),and the relative standard deviation of 45 volatile ovganic compounds was 3.8% - 15.8%. The average recovery was 79.3% - 119.0%. Conclusion: The method is simple,accurate,sensitive,has good separation effect,short analysis period, can be used for qualitative and quantitative analysis of volatile organic compounds in the workplace, and also supports the rapid identification and detection of occupational hazards.

Experimental and theoretical characterization of organic salt: 2-((4-bromophenyl)amino) pyrido[1,2-a] quinoxalin-11-ium bromide monohydrate synthesized via oxidative cyclization

NASA Astrophysics Data System (ADS)

Faizi, Md. Serajul Haque; Alam, Mohammad Jane; Haque, Ashanul; Ahmad, Shabbir; Shahid, M.; Ahmad, Musheer

2018-03-01

Quinoxalines are nitrogen-embedded heterocyclic compounds that possess unique and versatile pharmacological applications. The present article describes synthesis and characterization of organic salt 2-((4-bromophenyl)amino)pyrido [1,2-a]quinoxalin-11-ium bromide (BAPQ), an oxidative cyclized product of N-phenyl-N-(pyridine-2-ylmethylene)benzene-1,4-diamine (PPMD). The structure of the synthesized product was extensively characterized by 1H NMR, 2D-COSY NMR, MS, IR, UV-vis, X-ray techniques and elemental analysis. The electronic and structural properties of BAPQ was well complemented by performing extensive computational studies (B3LYP/6-311G (d,p) basis sets). Metal-free, mild reaction condition, easy work-up and excellent yield with high purity are main features of this work and thus holds promise for the generation of new compounds of this class. Analytical results indicated ionic nature of the compound with bromide as counterion. DFT calculation showed low kinetic stability and high reactivity of the compound.

Efficient synthesis and physicochemical characterization of natural danshensu, its S isomer and intermediates thereof

NASA Astrophysics Data System (ADS)

Sidoryk, Katarzyna; Filip, Katarzyna; Cmoch, Piotr; Łaszcz, Marta; Cybulski, Marcin

2018-02-01

The synthesis and molecular structure details of R- 3,4-dihydroxyphenyl lactic acid (danshensu) and related compounds, i.e. S isomer and the key intermediates have been described. Danshensu is an important water soluble phenolic acid of Salvia miltiorrhiza herb (danshen or red sag) with numerous applications in traditional Chinese medicine (TCM). Our synthetic approach was based on the Knoevenagel condensation of the protected 3,4-dihydroxybenzaldehyd and Meldrum acid derivative, followed by asymmetric Sharples dihydroxylation, reductive mono dehydroxylation and final deprotection. All compounds were characterized by various spectroscopic techniques: 1H-, 13C- magnetic resonance (NMR); Fourier-transformed infrared (FTIR); Raman, HR mass spectroscopy. For the determination of compound optical purities original HPLC methods were developed which allowed for the efficient resolution of danshensu R and S enantiomers as well as its intermediate enantiomers, using commercially available chiral stationary phases. Furthermore, in order to better understand danshensu specificity as a potential API in drug formulation, the physicochemical properties of the compounds were studied by thermal analysis, including differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA).

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

Highly enantioselective synthesis of γ-, δ-, and ε-chiral 1-alkanols via Zr-catalyzed asymmetric carboalumination of alkenes (ZACA)–Cu- or Pd-catalyzed cross-coupling

PubMed Central

Xu, Shiqing; Oda, Akimichi; Kamada, Hirofumi; Negishi, Ei-ichi

2014-01-01

Despite recent advances of asymmetric synthesis, the preparation of enantiomerically pure (≥99% ee) compounds remains a challenge in modern organic chemistry. We report here a strategy for a highly enantioselective (≥99% ee) and catalytic synthesis of various γ- and more-remotely chiral alcohols from terminal alkenes via Zr-catalyzed asymmetric carboalumination of alkenes (ZACA reaction)–Cu- or Pd-catalyzed cross-coupling. ZACA–in situ oxidation of tert-butyldimethylsilyl (TBS)-protected ω-alkene-1-ols produced both (R)- and (S)-α,ω-dioxyfunctional intermediates (3) in 80–88% ee, which were readily purified to the ≥99% ee level by lipase-catalyzed acetylation through exploitation of their high selectivity factors. These α,ω-dioxyfunctional intermediates serve as versatile synthons for the construction of various chiral compounds. Their subsequent Cu-catalyzed cross-coupling with various alkyl (primary, secondary, tertiary, cyclic) Grignard reagents and Pd-catalyzed cross-coupling with aryl and alkenyl halides proceeded smoothly with essentially complete retention of stereochemical configuration to produce a wide variety of γ-, δ-, and ε-chiral 1-alkanols of ≥99% ee. The MαNP ester analysis has been applied to the determination of the enantiomeric purities of δ- and ε-chiral primary alkanols, which sheds light on the relatively undeveloped area of determination of enantiomeric purity and/or absolute configuration of remotely chiral primary alcohols. PMID:24912191

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).

Impact of the uranium (VI) speciation in mineralised urines on its extraction by calix[6]arene bearing hydroxamic groups used in chromatography columns.

PubMed

Baghdadi, S; Bouvier-Capely, C; Ritt, A; Peroux, A; Fevrier, L; Rebiere, F; Agarande, M; Cote, G

2015-11-01

Actinides determination in urine samples is part of the analyses performed to monitor internal contamination in case of an accident or a terrorist attack involving nuclear matter. Mineralisation is the first step of any of these analyses. It aims at reducing the sample volume and at destroying all organic compounds present. The mineralisation protocol is usually based on a wet ashing step, followed by actinides co-precipitation and a furnace ashing step, before redissolution and the quantification of the actinides by the appropriate techniques. Amongst the existing methods to perform the actinides co-precipitation, alkali-earth (typically calcium) precipitation is widely used. In the present work, the extraction of uranium(VI), plutonium(IV) and americium(III) from the redissolution solutions (called "mineralised urines") on calix[6]arene columns bearing hydroxamic groups was investigated as such an extraction is a necessary step before their determination by ICP-MS or alpha spectrometry. Difficulties were encountered in the transfer of uranium(VI) from raw to mineralised urines, with yield of transfer ranging between 0% and 85%, compared to about 90% for Pu and Am, depending on the starting raw urines. To understand the origin of such a difficulty, the speciation of uranium (VI) in mineralised urines was investigated by computer simulation using the MEDUSA software and the associated HYDRA database, compiled with recently published data. These calculations showed that the presence of phosphates in the "mineralised urines" leads to the formation of strong uranyl-phosphate complexes (such as UO2HPO4) which compete with the uranium (VI) extraction by the calix[6]arene bearing hydroxamic groups. The extraction constant of uranium (VI) by calix[6]arene bearing hydroxamic groups was determined in a 0.04 mol L(-1) sodium nitrate solution (logK=4.86±0.03) and implemented in an extraction model taking into account the speciation in the aqueous phase. This model allowed to simulate satisfactorily the experimental uranium extraction data and to support the preliminary conclusions about the role of the phosphates present in mineralised urines. These calculations also showed that the phosphate/calcium ratio is a key parameter as far as the efficiency of the uranium (VI) extraction by the calix[6]arene columns is concerned. It predicted that the addition of CaCl2 in mineralised urines would release uranium (VI) from phosphates by forming calcium (II)-phosphate complexes and thus facilitate the uranium (VI) extraction on calix[6]arene columns. These predictions were confirmed experimentally as the addition of 0.1 mol L(-1) CaCl2 to a mineralised urine containing naturally a high concentration of phosphate (typically 0.04 mol L(-1)) significantly increased the percentage of uranium (VI) extraction on the calix[6]arene columns. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparative isolation and purification of harpagoside and angroside C from the root of Scrophularia ningpoensis Hemsley by high-speed counter-current chromatography.

PubMed

Tian, Jinfeng; Ye, Xiaoli; Shang, Yuanhong; Deng, Yafei; He, Kai; Li, Xuegang

2012-10-01

In this study, the bioactive component harpagoside and angroside C in the root of Scrophularia ningpoensis Hemsley was simultaneously separated by high-speed counter-current chromatography (HSCCC). A two-phase solvent system containing chloroform/n-butanol/methanol/water (4:1:3:2, v/v/v/v) was selected following consideration of the partition coefficient of the target compound. The crude extract (200 mg) was loaded onto a 280-mL HSCCC column and yielded 22 mg harpagoside and 31 mg angroside C with the purity of higher than 98 and 98.5%, respectively. It is feasible to isolate active compounds harpagoside and angroside C from S. ningpoensis using HSCCC. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

METHOD FOR PREPARING NORMORPHINE

DOEpatents

Rapoport, H.; Look, M.

1959-06-01

An improved method is presented for producing normorphine from morphine. Morphine as the starting material is acetylated by treatment with acetylating agents to produce di-acetyl morphine (heroin). The acetylated compound is reacted with cyanating agents to produce di-acetyl-cyanonormorphine (cyanonorheroin). The di-acetyl-cyanonormorphine compound is then treated in accordance with the improved hydrolysis reactions of the present invention in which concentrated hydrochloric acid is employed for a limited time period to hydrolyze the acetyl group therefrom forming cyanonormorphine. Subsequently, the reaction mixture is diluted and hydrolysis of the cyano groups from the cyanonormorphine is effected with a longer contact time with dilute hydrochloric acid thereby producing normorphine. A high over-all conversion and production of a high purity product which may be radioactlvely labeled, if desired, is obtained by operation of the process.

High temperature compounds for turbine vanes

NASA Technical Reports Server (NTRS)

Rhodes, W. H.; Cannon, R. M., Jr.

1972-01-01

Fabrication and microstructure control studies were conducted on SiC, Si3N4, and composites based on these compounds. Charpy mode impact testing to 2400 F established that beta-spodumene, lithium aluminum silicate, coated Si3N4, Si3N4 derived from alpha-Si3N4 powder, and SiC containing 5-25 v/o chopped C fibers had the most promising strengths. Several other composite systems had excellent microstructures and could prove interesting materials in the future. Stress-rupture testing on Si3N4 established that increasing 2000 F - 100 hour strengths were obtained for increasing grain size to at least 5 micrometers, increasing density and possibly increasing phase purity. These parameters became less important at 2400 F where it is thought a grain boundary phase controls strength.

Separation and purification of four flavonol diglucosides from the flower of Meconopsis integrifolia by high-speed counter-current chromatography.

PubMed

Huang, Yanfei; Han, Yatao; Chen, Keli; Huang, Bisheng; Liu, Yuan

2015-12-01

Flavonoids are the main components of Meconopsis integrifolia (Maxim.) Franch, which is a traditional Tibetan medicine. However, traditional chromatography separation requires a large quantity of raw M. integrifolia and is very time consuming. Herein, we applied high-speed counter-current chromatography in the separation and purification of flavonoids from the ethanol extracts of M. integrifolia flower. Ethyl acetate/n-butanol/water (2:3:5, v/v/v) was selected as the optimum solvent system to purify the four components, namely quercetin-3-O-β-d-glucopyrannosy-(1→6)-β-d-glucopyranoside (compound 1, 60 mg), quercetin 3-O-[2'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 2, 40 mg), quercetin 3-O-[3'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 3, 11 mg), and quercetin 3-O-[6'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 4, 16 mg). Among the four compounds, 3 and 4 were new acetylated flavonol diglucosides. After the high-speed counter-current chromatography separation, the purities of the four flavonol diglucosides were 98, 95, 90, and 92%, respectively. The structures of these compounds were identified by mass spectrometry and NMR spectroscopy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Margaret A. Marshall; John D. Bess; Yevgeniy Rozhikhin

In the early 1970s Dr. John T. Mihalczo (team leader), J.J. Lynn, and J.R. Taylor performed experiments at the Oak Ridge Critical Experiments Facility (ORCEF) with highly enriched uranium (HEU) metal (called Oak Ridge Alloy or ORALLOY) in an attempt to recreate GODIVA I results with greater accuracy than those performed at Los Alamos National Laboratory in the 1950s (HEU-MET-FAST-001). The purpose of the Oak Ridge ORALLOY Sphere (ORSphere) experiments was to estimate the unreflected and unmoderated critical mass of an idealized sphere of uranium metal corrected to a density, purity, and enrichment such that it could be compared withmore » the GODIVA I experiments[1]. Part of the experimental series was the measurement of the delayed neutron fraction, ßeff, using time correlation measurements and using the central void reactivity measurement. The time correlations measurements were rejected by the experimenter. The measurements using the central void reactivity measurement yielded a ßeff value of 0.00657, which agrees well with the value measured with GODIVA I (0.0066). This measurement is evaluated, found to be acceptable, and discussed in extensive detail in “ORSphere: Physics Measurements for Bare, HEU(93.2) Metal Sphere”[2]. In order to determine the delayed neutron fraction using the central void reactivity delayed neutron parameters must be used. The experimenter utilized the delayed neutron parameters set forth by Keepin, Wimment, and Zeigler[3]. If the derivation of the ßeff is repeated with different delayed neutron parameters from various modern nuclear data sets the resulting values vary greatly from the expected results.« less

Determination of the Secondary Neutron Flux at the Massive Natural Uranium Spallation Target

NASA Astrophysics Data System (ADS)

Zeman, M.; Adam, J.; Baldin, A. A.; Furman, W. I.; Gustov, S. A.; Katovsky, K.; Khushvaktov, J.; Mar`in, I. I.; Novotny, F.; Solnyshkin, A. A.; Tichy, P.; Tsoupko-Sitnikov, V. M.; Tyutyunnikov, S. I.; Vespalec, R.; Vrzalova, J.; Wagner, V.; Zavorka, L.

The flux of secondary neutrons generated in collisions of the 660 MeV proton beam with the massive natural uranium spallation target was investigated using a set of monoisotopic threshold activation detectors. Sandwiches made of thin high-purity Al, Co, Au, and Bi metal foils were installed in different positions across the whole spallation target. The gamma-ray activity of products of (n,xn) and other studied reactions was measured offline with germanium semiconductor detectors. Reaction yields of radionuclides with half-life exceeding 100 min and with effective neutron energy thresholds between 3.6 MeV and 186 MeV provided us with information about the spectrum of spallation neutrons in this energy region and beyond. The experimental neutron flux was determined using the measured reaction yields and cross-sections calculated with the TALYS 1.8 nuclear reaction program and INCL4-ABLA event generator of MCNP6. Neutron spectra in the region of activation sandwiches were also modeled with the radiation transport code MCNPX 2.7. Neutron flux based on excitation functions from TALYS provides a reasonable description of the neutron spectrum inside the spallation target and is in good agreement with Monte-Carlo predictions. The experimental flux that uses INCL4 cross-sections rather underestimates the modeled spectrum in the whole region of interest, but the agreement within few standard deviations was reached as well. The paper summarizes basic principles of the method for determining the spectrum of high-energy neutrons without employing the spectral adjustment routines and points out to the need for model improvements and precise cross-section measurements.

Molecular marker and stable carbon isotope analyses of carbonaceous Ambassador uranium ores of Mulga Rock in Western Australia

NASA Astrophysics Data System (ADS)

Jaraula, C.; Schwark, L.; Moreau, X.; Grice, K.; Bagas, L.

2013-12-01

Mulga Rock is a multi-element deposit containing uranium hosted by Eocene peats and lignites deposited in inset valleys incised into Permian rocks of the Gunbarrel Basin and Precambrian rocks of the Yilgarn Craton and Albany-Fraser Orogen. Uranium readily adsorbs onto minerals or phytoclasts to form organo-uranyl complexes. This is important in pre-concentrating uranium in this relatively young ore deposit with rare uraninite [UO2] and coffinite [U(SiO4)1-x(OH)4x], more commonly amorphous and sub-micron uranium-bearing particulates. Organic geochemical and compound-specific stable carbon isotope analyses were conducted to identify possible associations of molecular markers with uranium accumulation and to recognize effect(s) of ionizing radiation on molecular markers. Samples were collected from the Ambassador deposit containing low (<200 ppm) to high (>2000 ppm) uranium concentrations. The bulk rock C/N ratios of 82 to 153, Rock-Eval pyrolysis yields of 316 to 577 mg hydrocarbon/g TOC (Hydrogen Index, HI) and 70 to 102 mg CO2/g TOC (Oxygen Index, OI) are consistent with a terrigenous and predominantly vascular plant OM source deposited in a complex shallow water system, ranging from lacustrine to deltaic, swampy wetland and even shallow lake settings as proposed by previous workers. Organic solvent extracts were separated into saturated hydrocarbon, aromatic hydrocarbon, ketone, and a combined free fatty acid and alcohol fraction. The molecular profiles appear to vary with uranium concentration. In samples with relatively low uranium concentrations, long-chain n-alkanes, alcohols and fatty acids derived from epicuticular plant waxes dominate. The n-alkane distributions (C27 to C31) reveal an odd/even preference (Carbon Preference Index, CPI=1.5) indicative of extant lipids. Average δ13C of -27 to -29 ‰ for long-chain n-alkanes is consistent with a predominant C3 plant source. Samples with relatively higher uranium concentrations contain mostly intermediate-length n-alkanes, ketones, alcohols, and fatty acids (C20 to C24) with no preferential distribution (CPI~1). Intermediate length n-alkanes have modest carbon isotope enrichment compared to long-chain n-alkanes. These shorter-chain hydrocarbons are interpreted to represent alteration products. The diversity and relative abundance of ketones in highly mineralised Mulga Rock peats and lignites are not consistent with aerobic and diagenetic degradation of terrigenous OM in oxic environments. Moreover, molecular changes cannot be associated with thermal breakdown due to the low maturity of the deposits. It is possible that the association of high uranium concentrations and potential radiolysis resulted in the oxidation of alcohol functional groups into aldehydes and ketones and breakdown of highly aliphatic macromolecules (i.e. spores, pollen, cuticles, and algal cysts). These phytoclasts are usually considered to be recalcitrant as they evolved to withstand chemical and physical degradation. Previous petrographic analyses show that spores, pollen and wood fragments are preferentially enriched in uranium. Their molecular compositions are feasible sources of short- to intermediate-length n-alkanes that dominate the mineralised peats and lignites.

Development, upscaling and validation of the purification process for human-cl rhFVIII (Nuwiq®), a new generation recombinant factor VIII produced in a human cell-line.

PubMed

Winge, Stefan; Yderland, Louise; Kannicht, Christoph; Hermans, Pim; Adema, Simon; Schmidt, Torben; Gilljam, Gustav; Linhult, Martin; Tiemeyer, Maya; Belyanskaya, Larisa; Walter, Olaf

2015-11-01

Human-cl rhFVIII (Nuwiq®), a new generation recombinant factor VIII (rFVIII), is the first rFVIII produced in a human cell-line approved by the European Medicines Agency. To describe the development, upscaling and process validation for industrial-scale human-cl rhFVIII purification. The purification process involves one centrifugation, two filtration, five chromatography columns and two dedicated pathogen clearance steps (solvent/detergent treatment and 20 nm nanofiltration). The key purification step uses an affinity resin (VIIISelect) with high specificity for FVIII, removing essentially all host-cell proteins with >80% product recovery. The production-scale multi-step purification process efficiently removes process- and product-related impurities and results in a high-purity rhFVIII product, with an overall yield of ∼50%. Specific activity of the final product was >9000 IU/mg, and the ratio between active FVIII and total FVIII protein present was >0.9. The entire production process is free of animal-derived products. Leaching of potential harmful compounds from chromatography resins and all pathogens tested were below the limit of quantification in the final product. Human-cl rhFVIII can be produced at 500 L bioreactor scale, maintaining high purity and recoveries. The innovative purification process ensures a high-purity and high-quality human-cl rhFVIII product with a high pathogen safety margin. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

[Isolation and purification of seven catechin compounds from fresh tea leaves by semi-preparative liquid chromatography].

PubMed

Gong, Zhihong; Chen, Si; Gao, Jiangtao; Li, Meihong; Wang, Xiaxia; Lin, Jun; Yu, Xiaomin

2017-11-08

An effective and simple method was established to simultaneously purify seven tea catechins (gallocatechin (GC), epigallocatechin (EGC), catechin (C), epigallocatechin-3- O -gallate (EGCG), epicatechin (EC), epigallocatechin-3- O -(3- O -methyl)-gallate (EGCG3"Me) and epicatechin-3- O -gallate (ECG)) from fresh tea leaves by semi-preparative high performance liquid chromatography (HPLC). Fresh leaves of Tieguanyin tea were successively extracted with methanol and chloroform. Then crude catechins were precipitated from the aqueous fraction of chloroform extraction by adding lead subacetate. Crude catechins were used for the isolation of the seven target catechin compounds by semi-preparative HPLC. Methanol-water and acetonitrile-water were sequentially used as mobile phases. After two rounds of semi-preparative HPLC, all target compounds were achieved with high purities (>90%). The proposed method was tested on two additional tea cultivars and showed similar results. This method demonstrated a simple and efficient strategy based on solvent extraction, ion precipitation and semi-preparative HPLC for the preparation of multiple catechins from tea leaves.

Structural Elucidation of Novel Saponins in the Sea Cucumber Holothuria lessoni

PubMed Central

Bahrami, Yadollah; Zhang, Wei; Chataway, Tim; Franco, Chris

2014-01-01

Sea cucumbers are prolific producers of a wide range of bioactive compounds. This study aimed to purify and characterize one class of compound, the saponins, from the viscera of the Australian sea cucumber Holothuria lessoni. The saponins were obtained by ethanolic extraction of the viscera and enriched by a liquid-liquid partition process and adsorption column chromatography. A high performance centrifugal partition chromatography (HPCPC) was applied to the saponin-enriched mixture to obtain saponins with high purity. The resultant purified saponins were profiled using MALDI-MS/MS and ESI-MS/MS which revealed the structure of isomeric saponins to contain multiple aglycones and/or sugar residues. We have elucidated the structure of five novel saponins, Holothurins D/E and Holothurinosides X/Y/Z, along with seven reported triterpene glycosides, including sulfated and non-sulfated saponins containing a range of aglycones and sugar moieties, from the viscera of H. lessoni. The abundance of novel compounds from this species holds promise for biotechnological applications. PMID:25110919

Preparation of a novel radiotracer targeting the EphB4 receptor via radiofluorination using spiro azetidinium salts as precursor.

PubMed

Wiemer, Jens; Steinbach, Jörg; Pietzsch, Jens; Mamat, Constantin

2017-08-01

The visualization of Eph receptors, which are overexpressed in various tumor entities, using selective small molecule Eph inhibitors by means of positron emission tomography is a promising approach for tumor imaging. N-(Pyrimidinyl)indazolamines represent a class of compounds, which are known to have high affinity especially for the EphB4 receptor. Radiofluorination of these compounds could provide a highly specific imaging agent and was investigated using a classical nucleophilic introduction of [ 18 F]fluoride as well as a less common nucleophilic ring-opening reaction of azetidinium salts. In the past, radiofluorinations using azetidinium precursors were demonstrated to result in high radiochemical yields in short periods. For this purpose, an azetidinium precursor based on the N-(pyrimidinyl)indazolamine lead compound was developed, and radiofluorination was successfully accomplished. The respective [ 18 F]radiotracer was quickly prepared with high radiochemical purity >97% and in a radiochemical yield of 34%. Copyright © 2017 John Wiley & Sons, Ltd.

OSL studies of alkali fluoroperovskite single crystals for radiation dosimetry

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Raja, A.; Madhusoodanan, U.; Annalakshmi, O.; Ramasamy, P.

2016-08-01

This paper presents a preliminary investigation of the optically stimulated luminescence (OSL) of alkali fluoroperovskite single crystals for radiation dosimetry. The perovskite-like KMgF3, NaMgF3 and LiBaF3 polycrystalline compounds doped with rare earths (Eu2+ and Ce3+) were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of these compounds have been grown from melt by using vertical Bridgman-Stockbarger method. The Linearly Modulated OSL and Continuous Wave OSL measurements were performed in these alkali fluorides using blue light stimulation. Thermal bleaching experiments have shown that OSL signals originate from traps which are unstable near 200 °C, thus proving the suitability of the signals for dosimetric purposes. Optical bleaching measurements were also performed for these fluoride samples. OSL dose response was studied as a function of dose which was found to increase with beta dose.

Sustainable production of valuable compound 3-succinoyl-pyridine by genetically engineering Pseudomonas putida using the tobacco waste.

PubMed

Wang, Weiwei; Xu, Ping; Tang, Hongzhi

2015-11-17

Treatment of solid and liquid tobacco wastes with high nicotine content remains a longstanding challenge. Here, we explored an environmentally friendly approach to replace tobacco waste disposal with resource recovery by genetically engineering Pseudomonas putida. The biosynthesis of 3-succinoyl-pyridine (SP), a precursor in the production of hypotensive agents, from the tobacco waste was developed using whole cells of the engineered Pseudomonas strain, S16dspm. Under optimal conditions in fed-batch biotransformation, the final concentrations of product SP reached 9.8 g/L and 8.9 g/L from aqueous nicotine solution and crude suspension of the tobacco waste, respectively. In addition, the crystal compound SP produced from aqueous nicotine of the tobacco waste in batch biotransformation was of high purity and its isolation yield on nicotine was 54.2%. This study shows a promising route for processing environmental wastes as raw materials in order to produce valuable compounds.

Ultrasonic promoted synthesis of novel s-triazine-Schiff base derivatives; molecular structure, spectroscopic studies and their preliminary anti-proliferative activities

NASA Astrophysics Data System (ADS)

El-Faham, Ayman; Soliman, Saied M.; Ghabbour, Hazem A.; Elnakady, Yasser A.; Mohaya, Talal A.; Siddiqui, Mohammed R. H.; Albericio, Fernando

2016-12-01

Novel series of s-triazine-Schiff base derivatives were synthesized employing ultrasonic irradiation and characterized by NMR (1H and 13C), FT-IR, and elemental analysis. The use of ultrasonic irradiation has allowed the preparation of the target products with better yields in shorter reaction time and excellent purities compared to the conventional heating. X-ray single crystal diffraction experiments verified the molecular structure of four from the new prepared s-triaizne-Schiff base derivatives. The molecular structures of the studied compounds are computerized using DFT/B3LYP method. The effects of substituent at the triazine and phenyl ring on the electronic and spectroscopic properties of the studied compounds were also investigated. The natural atomic charges showed that pipridino-s-triazine derivatives are richer in electrons than those having morpholino derivatives. The anti-proliferative effects for the prepared compounds were tested against three different cancer cell lines.

Separation of uranium isotopes by chemical exchange

DOEpatents

Ogle, P.R. Jr.

1974-02-26

A chemical exchange method is provided for separating /sup 235/U from / sup 238/U comprising contacting a first phase containing UF/sub 6/ with a second phase containing a compound selected from the group consisting of NOUF/sub 6/, NOUF/sub 7/, and NO/sub 2/UF/sub 7/ until the U Fsub 6/ in the first phase becomes enriched in the /sup 235/U isotope. (Official Gazette)

242-A Evaporator/plutonium uranium extraction (PUREX) effluent treatment facility (ETF) nonradioactive air emission test report

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

Hill, J.S., Westinghouse Hanford

1996-05-10

This report shows the methods used to test the stack gas outlet concentration and emission rate of Volatile Organic Compounds as Total Non-Methane Hydrocarbons in parts per million by volume,grams per dry standard cubic meter, and grams per minute from the PUREX ETF stream number G6 on the Hanford Site. Test results are shown in Appendix B.1.

Radiation- and Depleted Uranium-Induced Carcinogenesis Studies: Characterization of the Carcinogenic Process and Development of Medical Countermeasures

DTIC Science & Technology

2005-01-01

drug development. 3.2 Candidate Agents: Phenylacetate and Epigallocatechin Gallate Phenylacetate (PA) is an attractive candidate for our studies...The polyphenol, epigallocathechin-3 gallate ( EGCG ), a major constituent of green tea, is also an attractive candidate for low-dose radiation...preventive agents. Part 1: chemopreventive potential of Epigallocatechin gallate , cimigenol, cimigenol-3,15-dione, and related compounds, Bioorganic Medical

Maruhn-Greiner Maximum of Uranium Fission for Confirmation of Low Energy Nuclear Reactions LENR via a Compound Nucleus with Double Magic Numbers

NASA Astrophysics Data System (ADS)

Hora, H.; Miley, G. H.

2007-12-01

One of the most convincing facts about LENR due to deuterons of very high concentration in host metals as palladium is the measurement of the large scale minimum of the reaction probability depending on the nucleon number A of generated elements at A = 153 where a local maximum was measured. This is similar to the fission of uranium at A = 119 where the local maximum follows from the Maruhn-Greiner theory if the splitting nuclei are excited to about MeV energy. The LENR generated elements can be documented any time after the reaction by SIMS or K-shell X-ray excitation to show the very unique distribution with the local maximum. An explanation is based on the strong Debye screening of the Maxwellian deuterons within the degenerate rigid electron background especially within the swimming electron layer at the metal surface or at interfaces. The deuterons behave like neutrals at distances of about 2 picometers. They may form clusters due to soft attraction in the range above thermal energy. Clusters of 10 pm diameter may react over long time probabilities (megaseconds) with Pd nuclei leading to a double magic number compound nucleus which splits like in fission to the A = 153 element distribution.

Compounding pharmacy conundrum: "we cannot live without them but we cannot live with them" according to the present paradigm.

PubMed

Guharoy, Roy; Noviasky, John; Haydar, Ziad; Fakih, Mohamad G; Hartman, Christian

2013-04-01

Compounding pharmacies serve a critical role in modern health care to meet special patient care needs. Although the US Food and Drug Administration (FDA) has clearly delineated jurisdiction over drug companies and products manufactured under Good Manufacturing Practice (GMP) regulations to ensure quality, potency, and purity, compounding pharmacies are regulated by the State Boards and are not registered by the FDA. In recent years, some compounding pharmacies acted like a manufacturer, preparing large amounts of injectable drugs with interstate activities. Multiple outbreaks have been linked to compounding pharmacies, including a recent outbreak of fungal meningitis related to contaminated methylprednisolone, exposing > 14,000 patients in multiple states. This tragedy underscores the urgency of addressing safety related to compounding pharmacies. There is a call for action at the federal and state levels to set minimum production standards, impose new labeling conditions on compounded drugs, and require large-scale compounders be regulated by the FDA. "Industrial" compounding must come under FDA oversight, require those pharmacies to meet GMP standards, and ensure quality and safe products for patient use. Moreover, compliance with the Institute for Safe Medication Practices 2011 recommendations that any type of sterile compounding must be in compliance with the United States Pharmacopoeia chapter 797 guidelines will reduce the risk of patient harm from microbial contamination. Finally, other critical factors that require close attention include addressing injectable products compounded in hospitals and other outpatient health-care centers. The FDA and State Boards of Pharmacy must be adequately funded to exercise the oversight effectively.

Direct dating of archaeological pottery by compound-specific 14C analysis of preserved lipids.

PubMed

Stott, Andrew W; Berstan, Robert; Evershed, Richard P; Bronk-Ramsey, Christopher; Hedges, Robert E M; Humm, Martin J

2003-10-01

A methodology is described demonstrating the utility of the compound-specific 14C technique as a direct means of dating archaeological pottery. The method uses automated preparative capillary gas chromatography employing wide-bore capillary columns to isolate individual compounds from lipid extracts of archaeological potsherds in high purity (>95%) and amounts (>200 microg) sufficient for radiocarbon dating using accelerator mass spectrometry (AMS). A protocol was developed and tested on n-alkanes and n-carboxylic acids possessing a broad range of 14C ages. Analytical blanks and controls allowed background 14C measurements to be assessed and potential sources of errors to be detected, i.e., contamination with modern or dead 14C, isotopic fraction effects, etc. A "Russian doll" method was developed to transfer isolated target compounds onto tin powder/capsules prior to combustion and AMS analyses. The major advantage of the compound-specific technique is that 14C dates obtained for individual compounds can be directly linked to the commodities processed in the vessels during their use, e.g., animal fats. The compound-specific 14C dating protocol was validated on a suite of ancient pottery whose predicted ages spanned a 5000-year date range. Initial results indicate that meaningful correlations can be obtained between the predicted date of pottery and that of the preserved lipids. These findings constitute an important step forward to the direct dating of archaeological pottery.

Molecular analysis of phosphate limitation in Geobacteraceae during the bioremediation of a uranium-contaminated aquifer

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

N'Guessan, L.A.; Elifantz, H.; Nevin, K.P.

2009-09-01

Nutrient limitation is an environmental stress that may reduce the effectiveness of bioremediation strategies, especially when the contaminants are organic compounds or when organic compounds are added to promote microbial activities such as metal reduction. Genes indicative of phosphate-limitation were identified via microarray analysis of chemostat cultures of Geobacter sulfureducens. This analysis revealed that genes in the pst-pho operon, which is associated with a high affinity phosphate uptake system in other microorganisms, had significantly higher transcript abundance under phosphate-limiting conditions, with the genes pstB and phoU the most up-regulated. Quantitative PCR analysis of pstB and phoU transcript levels in G.more » sulfurreducens grown in chemostats demonstrated that the expression of these genes increased when phosphate was removed from the culture medium. Transcripts of pstB and phoU within the subsurface Geobacter species predominating during an in situ uranium bioremediation field experiment were more abundant than in chemostat cultures of G. sulfurreducens that were not limited for phosphate. Addition of phosphate to incubations of subsurface sediments did not stimulate dissimilatory metal reduction. The added phosphate was rapidly adsorbed onto the sediments. The results demonstrate that Geobacter species can effectively reduce U(VI) even when experiencing suboptimal phosphate concentrations and that increasing phosphate availability with phosphate additions is difficult to achieve due to the high reactivity of this compound. This transcript-based approach developed for diagnosing phosphate limitation should be applicable to assessing the potential need for additional phosphate in other bioremediation processes.« less

Molecular Analysis of Phosphate Limitation in Geobacteraceae During the Bioremediation of a Uranium-Contaminated Aquifer

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

N'Guessan, A. Lucie; Elifantz, H.; Nevin, Kelly P.

2010-02-01

Nutrient limitation is an environmental stress that may reduce the effectiveness of bioremediation strategies, especially when the contaminants are organic compounds or when organic compounds are added to promote microbial activities such as metal reduction. Genes indicative of phosphate-limitation were identified via microarray analysis of chemostat cultures of Geobacter sulfureducens. This analysis revealed that genes in the pst-pho operon, which is associated with a high affinity phosphate uptake system in other microorganisms, had significantly higher transcript abundance under phosphate-limiting conditions, with the genes pstB and phoU the most up-regulated. Quantitative PCR analysis of pstB and phoU transcript levels in G.more » sulfurreducens grown in chemostats demonstrated that the expression of these genes increased when phosphate was removed from the culture medium. Transcripts of pstB and phoU within the subsurface Geobacter species predominating during an in situ uranium bioremediation field experiment were more abundant than in chemostat cultures of G. sulfurreducens that were not limited for phosphate. Addition of phosphate to incubations of subsurface sediments did not stimulate dissimilatory metal reduction. The added phosphate was rapidly adsorbed onto the sediments. The results demonstrate that Geobacter species can effectively reduce U(VI) even when experiencing suboptimal phosphate concentrations and that increasing phosphate availability with phosphate additions is difficult to achieve due to the high reactivity of this compound. This transcript-based approach developed for diagnosing phosphate limitation should be applicable to assessing the potential need for additional phosphate in other bioremediation processes.« less

Molecular analysis of phosphate limitation in Geobacteraceae during the bioremediation of a uranium-contaminated aquifer

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

N'Guessan, A. Lucie; Elifantz, H.; Nevin, Kelly P.

2010-01-10

Nutrient limitation is an environmental stress that may reduce the effectiveness of bioremediation strategies, especially when the contaminants are organic compounds or when organic compounds are added to promote microbial activities such as metal reduction. Genes indicative of phosphatelimitation were identified by microarray analysis of chemostat cultures of Geobacter sulfureducens. This analysis revealed that genes in the pst-pho operon, which is associated with a high-affinity phosphate uptake system in other microorganisms, had significantly higher transcript abundance under phosphate-limiting conditions, with the genes pstB and phoU upregulated the most. Quantitative PCR analysis of pstB and phoU transcript levels in G. sulfurreducensmore » grown in chemostats demonstrated that the expression of these genes increased when phosphate was removed from the culture medium. Transcripts of pstB and phoU within the subsurface Geobacter species predominating during an in situ uranium-bioremediation field experiment were more abundant than in chemostat cultures of G. sulfurreducens that were not limited for phosphate. Addition of phosphate to incubations of subsurface sediments did not stimulate dissimilatory metal reduction. The added phosphate was rapidly adsorbed onto the sediments. The results demonstrate that Geobacter species can effectively reduce U(VI) even when experiencing suboptimal phosphate concentrations and that increasing phosphate availability with phosphate additions is difficult to achieve because of the high reactivity of this compound. This transcript-based approach developed for diagnosing phosphate limitation should be applicable to assessing the potential need for additional phosphate in other bioremediation processes.« less

Demonstration and Validation of a Regenerated Cellulose Dialysis Membrane Diffusion Sampler for Monitoring Ground Water Quality and Remediation Progress at DoD Sites for Perchlorate and Explosives Compounds (ER-0313)

DTIC Science & Technology

2010-09-30

Inductively coupled plasma – mass spectrometry ITRC Interstate Technology Regulatory Council LRL Laboratory reporting level LDPE Low-density polyethylene...diameter of the well. Another diffusion membrane sampler design consists of a tubular-shaped bag made of flexible low-density polyethylene ( LDPE ...Vroblesky, 2001a, 2001b). The LDPE tube is heat-sealed on one end, filled with high-purity water, heat-sealed at the top, and then suspended in a well to

Preparation of Radiolabeled Compounds for the U.S. Army Drug Development Program.

DTIC Science & Technology

1996-12-01

with borane -THF complex gave an 83% radiochemical yield of [14C]-19 after several recrystallizations from ethanol. In the master synthesis , alcohol...amide [14C]-15 in 88% radiochemical yield and 99% radiochemical purity after chromatography. Reduction of [14C]-15 with borane -THF complex afforded a...163 mCi) and tetrahydrofuran (freshly distilled) (28.6 mL) in a 1 00-mL RBF was cooled to 0 0C by an ice-bath. Borane -tetra- hydrofuran complex (10.8 mL

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloranisole

DOEpatents

Ott, Donald G.; Benziger, Theodore M.

1990-01-01

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloroanisole

DOEpatents

Ott, Donald G.; Benziger, Theodore M.

1991-01-01

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.

Purification of organic nonlinear optical materials for bulk crystal growth from melt

NASA Astrophysics Data System (ADS)

Gebre, Tesfaye; Bhat, Kamala N.; Batra, Ashok K.; Lal, Ravindra B.; Aggarwal, Mohan D.; Penn, Benjamin G.; Frazier, Donald O.

2002-10-01

The techniques developed for purification of nonlinear optical organic materials, such as benzil, 2-methyl-4-nitroaniline (MNA), Dicyanovinyl anisole (DIVA) and its derivatives, nitrophenyl prolinol (NPP) and other Schiff's base compounds, include Kugelrohy method, physical vapor transport, zone refining and recrystallization from the solvent are described. Purity of the materials is tested using differential thermal analysis, gas chromatograph/Mass detector, Fourier Transform Infrared spectroscopy and melting point measurements. The purified materials were later used in the growth of single crystal by Bridgman-Stockbarger and Czochralski techniques.

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloroanisole

DOEpatents

Ott, D.G.; Benziger, T.M.

1991-03-05

Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole is described. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB. 8 figures.

Effect of ZrO2 Source Variations on PbZrO3 - PbTiO3 Piezoelectric Properties.

DTIC Science & Technology

1980-01-15

wfatevalatediohryand wetbnde led/1cn Dipatont aod blNdigohvrywssontoyedP- aeilwt Coe 71 Wsingtongq D roC., e 20390 dnit Z-T ID 5,RM 1473 EDITION OF CAIO NOVGADN...PZ-PT 19 D . Coprecipitation of PZ-PT 26 IV SUMMARY AND CONCLUSIONS 33 V ACKNOWLEDGEMENTS 34 46 0 I 347602V ! _ _ A List of Illustrations Figure Page 1...chloride solution may be processed further to give high-purity zirconium (or zirconyl) compounds, such as the oxide, fluoride, nitrate , sulfate and

SUMMARY TECHNICAL REPORT ON FEED MATERIALS FOR THE PERIOD APRIL 1, 1959 TO JUNE 30, 1959

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

Simmons, J.W. ed.

1959-07-20

Anaconda Acld, Kermac, Moab, Rifle, and Texas Zinc uranium concentrates were evaluated (the laboratory portlon of feed material evaluation). Laboratory equilibrium tests and Pilot Plant 2-inch-column extraction tests demonstrated effective distribution of uranium into a TBPkerosene solvent from aqueous phases containing as little as 0.5N HNO/sub 3/ and varying amounts of added metal nitrates (NaNO/sub 3/). The concentration of assoclated nitric acid in dilute aqueous nitric acld solutions was determined after values were obtained for the equillbrium constant for the reaction of tri-n-butyl phosphate with associated nitric acid and for the equilibrium distribution constant for the partition of associated nitricmore » acld into tri-n-butyl phosphate. Optimum partition of uranium into tri-n-butyl phosphate was realized in the laboratory by using an aqueous uranyl nitrate solution containing sufficient hydrogen ions to promote extraction and a low concentration of associated nitric acid. An Ohmart system for controlling the uranium profile in the A'' extractlon column was installed on Refinery pulse columns. Use of this system improved control but did not stop all column upsets. The effect of 13 to l89 ppm sodium contaminatlon upon hydrofluorination conversion of teraperature at the site of the reaction. Uranyl sulfate was shown to undergo an enantiotroplc transitlon at 755 deg C and to decompose to U/sub 3/O/sub 8/ in an atmosphere of oxygen sulfur dioxide, which gases are evolved during decoraposition. Decontamination of sodium, calcium, nickel, magnesium, gadolinium, and dysprosium was achieved in a laboratory investigatlon of the ADU process. UO/sub 2/ produced by reductions programmed from 700 to ll00 deg F was hydrofluorinated at programmed temperatures of 550 to 1100 deg F and isothermally at ll00 deg F. Good conversion was obtained for material whose source was ADU calcined at 1200 deg F. Uranium derbles were classified by the present method of derby grading and were then examined for slag coverage, slag volume, and slag weight. There was a high degree of overlap of these parameters for adjacent grades. A hydraulic separator for separatlng uranlum from magnesium and magnesium fluorlde was fabrlcated. Excellent separatlon was obtained for +l6 mesh material. A hydrochloric acid dissolution- UF/sub 4/ precipitation process for routing scrap materials to the reductlon-to- metal step was examined. The purification obtained was noted, and process conditions were varied to determine their effect upon UF/sub 4/ density, UF/sub 4/ purity and precipitation time. Three types of uranium scrap were subjected to the HCl dissolution-aqueous precipitation Winlo process to determine the purification achieved. Green salt made from dolomitlc bomb liner residues was found to be grossly contaminated. Acceptable green salt was raade from pickle liquor treated with formaldehyde and from pickle liquor plus black oxide. Nominal 80% yields were obtained in the recovery of magnesium metal by reaction of calcium carblde with magnesium fluoride slag and in the recovery of HF by the reactlon of sulfuric acid wlth magnesium fluoride slag. A sample holder for use in quantitative preferred orientation studies was fabricated. The holder, designed to fit a North American Philips Gonionweter, will accommodate specimens up to l 13/16 inches in diameter and incorporates a precision ball bearing. A satisfactory technique was developed for the analysis of uranium metal for traces of fluoride. A direct flame photometric method is glven for the determination of magnesium in uranium ore concentrates. No chemical separation step is required, except for high-iron-content ores. (auth)« less

Analysis and Purification of Bioactive Natural Products: The AnaPurNa Study

PubMed Central

2012-01-01

Based on a meta-analysis of data mined from almost 2000 publications on bioactive natural products (NPs) from >80 000 pages of 13 different journals published in 1998–1999, 2004–2005, and 2009–2010, the aim of this systematic review is to provide both a survey of the status quo and a perspective for analytical methodology used for isolation and purity assessment of bioactive NPs. The study provides numerical measures of the common means of sourcing NPs, the chromatographic methodology employed for NP purification, and the role of spectroscopy and purity assessment in NP characterization. A link is proposed between the observed use of various analytical methodologies, the challenges posed by the complexity of metabolomes, and the inescapable residual complexity of purified NPs and their biological assessment. The data provide inspiration for the development of innovative methods for NP analysis as a means of advancing the role of naturally occurring compounds as a viable source of biologically active agents with relevance for human health and global benefit. PMID:22620854

Preparative Isolation and Purification of Flavone C-Glycosides from the Leaves of Ficus microcarpa L. f by Medium-Pressure Liquid Chromatography, High-Speed Countercurrent Chromatography, and Preparative Liquid Chromatography

PubMed Central

Wang, Xiaohong; Liang, Yong; Zhu, Licai; Xie, Huichun; Li, Hang; He, Junting; Pan, Man; Zhang, Tianyou; Ito, Yoichiro

2009-01-01

Combined with medium-pressure liquid chromatography (MPLC) and preparative high-performance liquid chromatography (perp-HPLC), high-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavone C-glycosides from the crude extract of leaves of Ficus microcarpae L. f. HSCCC separation was performed on a two-phase solvent system composed of methyl tert- butyl ether - ethyl acetate – 1-butanol – acetonitrile – 0.1% aqueous trifluoroacetic acid at a volume ratio of 1:3:1:1:5. Partially resolved peak fractions from HSCCC separation were further purified by preparative HPLC. Four well-separated compounds were obtained and their purities were determined by HPLC. The purities of these peaks were 97.28%, 97.20%, 92.23%, and 98.40%.. These peaks were characterized by ESI-MSn. According to the reference, they were identified as orientin (peak I), isovitexin-3″-O-glucopyranoside (peak II), isovitexin (peak III), and vitexin (peak IV), yielded 1.2 mg, 4.5 mg, 3.3 mg, and 1.8 mg, respectively. PMID:20190866

Separation of tartronic and glyceric acids by simulated moving bed chromatography.

PubMed

Coelho, Lucas C D; Filho, Nelson M L; Faria, Rui P V; Ferreira, Alexandre F P; Ribeiro, Ana M; Rodrigues, Alírio E

2018-08-17

The SMB unit developed by the Laboratory of Separation and Reaction Engineering (FlexSMB-LSRE ® ) was used to perform tartronic acid (TTA) and glyceric acid (GCA) separation and to validate the mathematical model in order to determine the optimum operating parameters of an industrial unit. The purity of the raffinate and extract streams in the experiments performed were 80% and 100%, respectively. The TTA and GCA productivities were 79 and 115 kg per liter of adsorbent per day, respectively and only 0.50 cubic meters of desorbent were required per kilogram of products. Under the optimum operating conditions, which were determined through an extensive simulation study based on the mathematical model developed to predict the performance of a real SMB unit, it was possible to achieve a productivity of 86 kg of TTA and 176 kg of GCA per cubic meter of adsorbent per day (considering the typical commercial purity value of 97% for both compounds) with an eluent consumption of 0.30 cubic meters per kilogram of products. Copyright © 2018 Elsevier B.V. All rights reserved.

Chlorine effect on the formation of carbon nanofibers.

PubMed

Lin, Wang-Hua; Takahashi, Yusuke; Li, Yuan-Yao; Sakoda, Akiyoshi

2012-12-01

Platelet graphite nanofibers (GNFs) and turbostratic carbon nanofibers (CNFs) are synthesized by the thermal evaporation and decomposition of a polymer-based mixture at 700 degrees C using Ni as a catalyst. The mixture consists of poly(ethylene glycol) (PEG), serving as the carbon source, and hydrochloric acid solution (HCl(aq)), serving as the promoter/additive for the growth of CNFs. High-purity zigzag-shaped platelet GNFs form with 10 wt% HCl(aq) as an additive in the PEG. The diameters of the platelet GNFs are in the range of 40-60 nm, with lengths of a few micrometers. High-resolution transmission electron microscopy images indicate a high degree of graphitization and well ordered graphene layers along the fiber axis. In contrast, high-purity turbostratic CNFs form with 20 wt% HCl(aq) in the PEG. The diameter and length of the turbostratic CNFs are 20-40 nm and a few micrometers, respectively. The participation of HCl in the thermal process leads to the formation of Ni-Cl compounds. The amount of chlorine affects the shape of the Ni catalyst, which determines the type of CNF formed.

Photochemical isotope separation

DOEpatents

Robinson, C. Paul; Jensen, Reed J.; Cotter, Theodore P.; Greiner, Norman R.; Boyer, Keith

1987-01-01

A process for separating isotopes by selective excitation of isotopic species of a volatile compound by tuned laser light. A highly cooled gas of the volatile compound is produced in which the isotopic shift is sharpened and defined. Before substantial condensation occurs, the cooled gas is irradiated with laser light precisely tuned to a desired wavelength to selectively excite a particular isotopic species in the cooled gas. The laser light may impart sufficient energy to the excited species to cause it to undergo photochemical reaction or even to photoionize. Alternatively, a two-photon irradiation may be applied to the cooled gas to induce photochemical reaction or photoionization. The process is particularly applicable to the separation of isotopes of uranium and plutonium.