Method for establishing a combustion zone in an in situ oil shale retort having a pocket at the top

DOEpatents

Cha, Chang Y.

1980-01-01

An in situ oil shale retort having a top boundary of unfragmented formation and containing a fragmented permeable mass has a pocket at the top, that is, an open space between a portion of the top of the fragmented mass and the top boundary of unfragmented formation. To establish a combustion zone across the fragmented mass, a combustion zone is established in a portion of the fragmented mass which is proximate to the top boundary. A retort inlet mixture comprising oxygen is introduced to the fragmented mass to propagate the combustion zone across an upper portion of the fragmented mass. Simultaneously, cool fluid is introduced to the pocket to prevent overheating and thermal sloughing of formation from the top boundary into the pocket.

Environmental research on a modified in situ oil shale task process. Progress report

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

Not Available

1980-05-01

This report summarizes the progress of the US Department of Energy's Oil Shale Task Force in its research program at the Occidental Oil Shale, Inc. facility at Logan Wash, Colorado. More specifically, the Task Force obtained samples from Retort 3E and Retort 6 and submitted these samples to a variety of analyses. The samples collected included: crude oil (Retort 6); light oil (Retort 6); product water (Retort 6); boiler blowdown (Retort 6); makeup water (Retort 6); mine sump water; groundwater; water from Retorts 1 through 5; retort gas (Retort 6); mine air; mine dust; and spent shale core (Retort 3E).more » The locations of the sampling points and methods used for collection and storage are discussed in Chapter 2 (Characterization). These samples were then distributed to the various laboratories and universities participating in the Task Force. For convenience in organizing the data, it is useful to group the work into three categories: Characterization, Leaching, and Health Effects. While many samples still have not been analyzed and much of the data remains to be interpreted, there are some preliminary conclusions the Task Force feels will be helpful in defining future needs and establishing priorities. It is important to note that drilling agents other than water were used in the recovery of the core from Retort 3E. These agents have been analyzed (see Table 12 in Chapter 2) for several constituents of interest. As a result some of the analyses of this core sample and leachates must be considered tentative.« less

Oil-shale program

NASA Astrophysics Data System (ADS)

Bader, B. E.

1981-10-01

The principal activities of the Sandia National Laboratories in the Department of Energy Oil shale program during the period April 1 to June 30, 1981 are discussed. Currently, Sandia's activities are focused upon: the development and use of analytical and experimental modeling techniques to describe and predict the retort properties and retorting process parameters that are important to the preparation, operation, and stability of in situ retorts, and the development, deployment, and field use of instrumentation, data acquisition, and process monitoring systems to characterize and evaluate in site up shale oil recovery operations. In-house activities and field activities (at the Geokinetics Oil Shale Project and the Occidental Oil Shale Project) are described under the headings: bed preparation, bed characterization, retorting process, and structural stability.

Withdrawal of gases and liquids from an in situ oil shale retort

DOEpatents

Siegel, Martin M.

1982-01-01

An in situ oil shale retort is formed within a subterranean formation containing oil shale. The retort contains a fragmented permeable mass of formation particles containing oil shale. A production level drift extends below the fragmented mass, leaving a lower sill pillar of unfragmented formation between the production level drift and the fragmented mass. During retorting operations, liquid and gaseous products are recovered from a lower portion of the fragmented mass. A liquid outlet line extends from a lower portion of the fragmented mass through the lower sill pillar for conducting liquid products to a sump in the production level drift. Gaseous products are withdrawn from the fragmented mass through a plurality of gas outlet lines distributed across a horizontal cross-section of a lower portion of the fragmented mass. The gas outlet lines extend from the fragmented mass through the lower sill pillar and into the production level drift. The gas outlet lines are connected to a gas withdrawal manifold in the production level drift, and gaseous products are withdrawn from the manifold separately from withdrawal of liquid products from the sump in the production level drift.

Method and apparatus for igniting an in situ oil shale retort

DOEpatents

Burton, Robert S.; Rundberg, Sten I.; Vaughn, James V.; Williams, Thomas P.; Benson, Gregory C.

1981-01-01

A technique is provided for igniting an in situ oil shale retort having an open void space over the top of a fragmented mass of particles in the retort. A conduit is extended into the void space through a hole in overlying unfragmented formation and has an open end above the top surface of the fragmented mass. A primary air pipe having an open end above the open end of the conduit and a liquid atomizing fuel nozzle in the primary air pipe above the open end of the primary air pipe are centered in the conduit. Fuel is introduced through the nozzle, primary air through the pipe, and secondary air is introduced through the conduit for vortical flow past the open end of the primary air pipe. The resultant fuel and air mixture is ignited for combustion within the conduit and the resultant heated ignition gas impinges on the fragmented mass for heating oil shale to an ignition temperature.

Method for rubblizing an oil shale deposit for in situ retorting

DOEpatents

Lewis, Arthur E.

1977-01-01

A method for rubblizing an oil shale deposit that has been formed in alternate horizontal layers of rich and lean shale, including the steps of driving a horizontal tunnel along the lower edge of a rich shale layer of the deposit, sublevel caving by fan drilling and blasting of both rich and lean overlying shale layers at the distal end of the tunnel to rubblize the layers, removing a substantial amount of the accessible rubblized rich shale to permit the overlying rubblized lean shale to drop to tunnel floor level to form a column of lean shale, performing additional sublevel caving of rich and lean shale towards the proximate end of the tunnel, removal of a substantial amount of the additionally rubblized rich shale to allow the overlying rubblized lean shale to drop to tunnel floor level to form another column of rubblized lean shale, similarly performing additional steps of sublevel caving and removal of rich rubble to form additional columns of lean shale rubble in the rich shale rubble in the tunnel, and driving additional horizontal tunnels in the deposit and similarly rubblizing the overlying layers of rich and lean shale and forming columns of rubblized lean shale in the rich, thereby forming an in situ oil shale retort having zones of lean shale that remain permeable to hot retorting fluids in the presence of high rubble pile pressures and high retorting temperatures.

Apparatus and method for igniting an in situ oil shale retort

DOEpatents

Chambers, Carlon C.

1981-01-01

A method and apparatus for conducting such method are disclosed for igniting a fragmented permeable mass of formation particles in an in situ oil shale retort. The method is conducted by forming a hole through unfragmented formation to the fragmented mass. An oxygen-containing gas is introduced into the hole. A fuel is introduced into a portion of the hole spaced apart from the fragmented mass. The fuel and oxygen-containing gas mix forming a combustible mixture which is ignited for establishing a combustion zone in a portion of the hole spaced apart from the fragmented mass. The hot gas generated in the combustion zone is conducted from the hole into the fragmented mass for heating a portion of the fragmented mass above an ignition temperature of oil shale.

Overview of the technology and status of oil sands development

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

Detamore, R.J.

1981-01-01

In conjunction with the increasing emphasis upon alternate energy sources, interest in the oil sands resource is discussed. This paper reviews the primary established oil sands recovery techniques including surface mining, surface retorting, in situ thermal and nonthermal in situ, and presents an overview of their application in specific projects.

Developing technologies for synthetic fuels

NASA Astrophysics Data System (ADS)

Sprow, F. B.

1981-05-01

After consideration of a likely timetable for the development of a synthetic fuels industry and its necessary supporting technology, the large variety of such fuels and their potential roles is assessed along with their commercialization outlook. Among the fuel production methods considered are: (1) above-ground retorting of oil shale; (2) in-situ shale retorting; (3) open pit mining of tar sands; (4) in-situ steam stimulation of tar sands; (5) coal gasification; (6) methanol synthesis from carbon monoxide and hydrogen; and (7) direct coal liquefaction by the hydrogenation of coal. It is shown that while the U.S. has very limited resource bases for tar sands and heavy crudes, the abundance of shale in the western states and the abundance and greater geographical dispersion of coal will make these the two most important resources of a future synthetic fuels industry.

Method for loading explosive laterally from a borehole

DOEpatents

Ricketts, Thomas E.

1981-01-01

There is provided a method for forming an in situ oil shale retort in a subterranean formation containing oil shale. At least one void is excavated in the formation, leaving zones of unfragmented formation adjacent the void. An array of main blastholes is formed in the zone of unfragmented formation and at least one explosive charge which is shaped for forming a high velocity gas jet is placed into a main blasthole with the axis of the gas jet extending transverse to the blasthole. The shaped charge is detonated for forming an auxiliary blasthole in the unfragmented formation adjacent a side wall of the main blasthole. The auxiliary blasthole extends laterally away from the main blasthole. Explosive is placed into the main blasthole and into the auxiliary blasthole and is detonated for explosively expanding formation towards the free face for forming a fragmented permeable mass of formation particles in the in situ oil shale retort.

Characterization of oil shale, isolated kerogen, and post-pyrolysis residues using advanced 13 solid-state nuclear magnetic resonance spectroscopy

USGS Publications Warehouse

Cao, Xiaoyan; Birdwell, Justin E.; Chappell, Mark A.; Li, Yuan; Pignatello, Joseph J.; Mao, Jingdong

2013-01-01

Characterization of oil shale kerogen and organic residues remaining in postpyrolysis spent shale is critical to the understanding of the oil generation process and approaches to dealing with issues related to spent shale. The chemical structure of organic matter in raw oil shale and spent shale samples was examined in this study using advanced solid-state 13C nuclear magnetic resonance (NMR) spectroscopy. Oil shale was collected from Mahogany zone outcrops in the Piceance Basin. Five samples were analyzed: (1) raw oil shale, (2) isolated kerogen, (3) oil shale extracted with chloroform, (4) oil shale retorted in an open system at 500°C to mimic surface retorting, and (5) oil shale retorted in a closed system at 360°C to simulate in-situ retorting. The NMR methods applied included quantitative direct polarization with magic-angle spinning at 13 kHz, cross polarization with total sideband suppression, dipolar dephasing, CHn selection, 13C chemical shift anisotropy filtering, and 1H-13C long-range recoupled dipolar dephasing. The NMR results showed that, relative to the raw oil shale, (1) bitumen extraction and kerogen isolation by demineralization removed some oxygen-containing and alkyl moieties; (2) unpyrolyzed samples had low aromatic condensation; (3) oil shale pyrolysis removed aliphatic moieties, leaving behind residues enriched in aromatic carbon; and (4) oil shale retorted in an open system at 500°C contained larger aromatic clusters and more protonated aromatic moieties than oil shale retorted in a closed system at 360°C, which contained more total aromatic carbon with a wide range of cluster sizes.

Hydrologic-information needs for oil-shale development, northwestern Colorado

USGS Publications Warehouse

Taylor, O.J.

1982-01-01

Hydrologic information is not adequate for proper development of the large oil-shale reserves of Piceance basin in northwestern Colorado. Exploratory drilling and aquifer testing are needed to define the hydrologic system, to provide wells for aquifer testing, to design mine-drainage techniques, and to explore for additional water supplies. Sampling networks are needed to supply hydrologic data on the quantity and quality of surface water, ground water, and springs. A detailed sampling network is proposed for the White River basin because of expected impacts related to water supplies and waste disposal. Emissions from oil-shale retorts to the atmosphere need additional study because of possible resulting corrosion problems and the destruction of fisheries. Studies of the leachate materials and the stability of disposed retorted shale piles are needed to insure that these materials will not cause problems. Hazards related to in-situ retorts, and the wastes related to oil-shale development in general also need further investigation. (USGS)

43 CFR 3922.20 - Application contents.

Code of Federal Regulations, 2011 CFR

2011-10-01

..., and transportation methods, including: (1) A description of the mining, retorting, or in situ mining... applications must be filed in the proper BLM State Office. No specific form of application is required, but the... is substantially identical to a technology or method currently in use to produce marketable...

43 CFR 3922.20 - Application contents.

Code of Federal Regulations, 2012 CFR

2012-10-01

..., and transportation methods, including: (1) A description of the mining, retorting, or in situ mining... applications must be filed in the proper BLM State Office. No specific form of application is required, but the... is substantially identical to a technology or method currently in use to produce marketable...

43 CFR 3922.20 - Application contents.

Code of Federal Regulations, 2013 CFR

2013-10-01

..., and transportation methods, including: (1) A description of the mining, retorting, or in situ mining... applications must be filed in the proper BLM State Office. No specific form of application is required, but the... is substantially identical to a technology or method currently in use to produce marketable...

43 CFR 3922.20 - Application contents.

Code of Federal Regulations, 2014 CFR

2014-10-01

..., and transportation methods, including: (1) A description of the mining, retorting, or in situ mining... applications must be filed in the proper BLM State Office. No specific form of application is required, but the... is substantially identical to a technology or method currently in use to produce marketable...

Leachate migration from an in-situ oil-shale retort near Rock Springs, Wyoming

USGS Publications Warehouse

Glover, Kent C.

1988-01-01

Hydrogeologic factors influencing leachate movement from an in-situ oil-shale retort near Rock Springs, Wyoming, were investigated through models of ground-water flow and solute transport. Leachate, indicated by the conservative ion thiocyanate, has been observed ? mile downgradient from the retort. The contaminated aquifer is part of the Green River Formation and consists of thin, permeable layers of tuff and sandstone interbedded with oil shale. Most solute migration has occurred in an 8-foot sandstone at the top of the aquifer. Ground-water flow in the study area is complexly three dimensional and is characterized by large vertical variations in hydraulic head. The solute-transport model was used to predict the concentration of thiocyanate at a point where ground water discharges to the land surface. Leachate with peak concentrations of thiocyanate--45 milligrams per liter or approximately one-half the initial concentration of retort water--was estimated to reach the discharge area during January 1985. This report describes many of th3 advantages, as well as the problems, of site-specific studies. Data such as the distribution of thin, permeable beds or fractures might introduce an unmanageable degree of complexity to basin-wide studies but can be incorporated readily into site-specific models. Solute migration in the study area occurs primarily in thin, permeable beds rather than in oil-shale strata. Because of this behavior, leachate traveled far greater distances than might otherwise have been expected. The detail possible in site-specific models permits more accurate prediction of solute transport than is possible with basin-wide models. A major problem in site-specific studies is identifying model boundaries that permit the accurate estimation of aquifer properties. If the quantity of water flowing through a study area cannot be determined prior to modeling, the hydraulic conductivity and ground-water velocity will be poorly estimated.

Leachate migration from an in situ oil-shale retort near Rock Springs, Wyoming

USGS Publications Warehouse

Glover, K.C.

1986-01-01

Geohydrologic factors influencing leachate movement from an in situ oil shale retort near Rock Springs, Wyoming, were investigated by developing models of groundwater flow and solute transport. Leachate, indicated by the conservative ion thiocyanate, has been observed 1/2 mi downgradient from the retort. The contaminated aquifer is part of the Green River Formation and consists of thin, permeable layers of tuff and sandstone interbedded with oil shale. Most solute migration has occurred in an 8-ft sandstone at the top of the aquifer. Groundwater flow in the study area is complexly 3-D and is characterized by large vertical variations in hydraulic head. The solute transport model was used to predict the concentration of thiocyanate at a point where groundwater discharges to the land surface. Leachates with peak concentrations of thiocyanate--45 mg/L or approximately one-half the initial concentration of retort water--were estimated to reach the discharge area during January 1985. Advantages as well as the problems of site specific studies are described. Data such as the distribution of thin permeable beds or fractures may introduce an unmanageable degree of complexity to basin-wide studies but can be incorporated readily in site specific models. Solute migration in the study area primarily occurs in thin permeable beds rather than in oil shale strata. Because of this behavior, leachate traveled far greater distances than might otherwise have been expected. The detail possible in site specific models permits more accurate prediction of solute transport than is possible with basin-wide models. A major problem in site specific studies is identifying model boundaries that permit the accurate estimation of aquifer properties. If the quantity of water flowing through a study area cannot be determined prior to modeling, the hydraulic conductivity and groundwater velocity will be estimated poorly. (Author 's abstract)

A feasibility study for high-temperature titanium reduction from TiCl4 using a magnesiothermic process

NASA Astrophysics Data System (ADS)

Ivanov, S. L.; Zablotsky, D.

2018-05-01

The current industrial practice for titanium extraction is a complex procedure, which produces a porous reaction mass of sintered titanium particulates fused to a steel retort wall with magnesium and MgCl2 trapped in the interstices. The reactor temperature is limited to approx. 900 °C due to the formation of fusible TiFe eutectic, which corrodes the retort and degrades the quality of titanium sponge. Here we examine the theoretical foundations and technological possibilities to design a shielded retort of niobium-zirconium alloy NbZr(1%), which is resistant to corrosion by titanium at high temperature. We consider the reactor at a temperature of approx. 1150 °C. Supplying stoichiometric quantities of reagents enables the reaction in the gas phase, whereas the exothermic process sustains the combustion of the reaction zone. When the pathway to the condenser is open, vacuum separation and evacuation of vaporized magnesium dichloride and excess magnesium into the water-cooled condenser take place. As both the reaction and the evacuation occur within seconds, the yield of the extraction is improved. We anticipate new possibilities for designing a device combining the retort function to conduct the reduction in the gas phase with fast vacuum separation of the reaction products and distillation of magnesium dichloride.

Method for in situ heating of hydrocarbonaceous formations

DOEpatents

Little, William E.; McLendon, Thomas R.

1987-01-01

A method for extracting valuable constituents from underground hydrocarbonaceous deposits such as heavy crude tar sands and oil shale is disclosed. Initially, a stratum containing a rich deposit is hydraulically fractured to form a horizontally extending fracture plane. A conducting liquid and proppant is then injected into the fracture plane to form a conducting plane. Electrical excitations are then introduced into the stratum adjacent the conducting plate to retort the rich stratum along the conducting plane. The valuable constituents from the stratum adjacent the conducting plate are then recovered. Subsequently, the remainder of the deposit is also combustion retorted to further recover valuable constituents from the deposit. Various R.F. heating systems are also disclosed for use in the present invention.

Migration through soil of organic solutes in an oil-shale process water

USGS Publications Warehouse

Leenheer, J.A.; Stuber, H.A.

1981-01-01

The migration through soil of organic solutes in an oil-shale process water (retort water) was studied by using soil columns and analyzing leachates for various organic constituents. Retort water extracted significant quantities of organic anions leached from ammonium-saturated-soil organic matter, and a distilled-water rinse, which followed retort-water leaching, released additional organic acids from the soil. After being corrected for organic constitutents extracted from soil by retort water, dissolved-organic-carbon fractionation analyses of effluent fractions showed that the order of increasing affinity of six organic compound classes for the soil was as follows: hydrophilic neutrals nearly equal to hydrophilic acids, followed by the sequence of hydrophobic acids, hydrophilic bases, hydrophobic bases, and hydrophobic neutrals. Liquid-chromatographic analysis of the aromatic amines in the hydrophobic- and hydrophilic-base fractions showed that the relative order of the rates of migration through the soil column was the same as the order of migration on a reversed-phase, octadecylsilica liquid-chromatographic column.

The role of water in unconventional in situ energy resource extraction technologies: Chapter 7 in Food, energy, and water: The chemistry connection

USGS Publications Warehouse

Gallegos, Tanya J.; Bern, Carleton R.; Birdwell, Justin E.; Haines, Seth S.; Engle, Mark A.

2015-01-01

Global trends toward developing new energy resources from lower grade, larger tonnage deposits that are not generally accessible using “conventional” extraction methods involve variations of subsurface in situ extraction techniques including in situ oil-shale retorting, hydraulic fracturing of petroleum reservoirs, and in situ recovery (ISR) of uranium. Although these methods are economically feasible and perhaps result in a smaller above-ground land-use footprint, there remain uncertainties regarding potential subsurface impacts to groundwater. This chapter provides an overview of the role of water in these technologies and the opportunities and challenges for water reuse and recycling.

Determining Permissible Oxygen and Water Vapor Transmission Rate for Non-Retort Military Ration Packaging

DTIC Science & Technology

2011-11-01

OXYGEN AND WATER VAPOR TRANSMISSION RATE FOR NON- RETORT MILITARY RATION PACKAGING by Danielle Froio Alan Wright Nicole Favreau and Sarah...ANSI Std. Z39.18 RETORT STORAGE SHELF LIFE RETORT POUCHES SENSORY ANALYSIS OXYGEN CRACKERS PACKAGING SENSORY... Packaging for MRE. (a) MRE Retort Pouch Quad-Laminate Structure; (b) MRE Non- retort Pouch Tri-Laminate Structure

Solar retorting of oil shale

DOEpatents

Gregg, David W.

1983-01-01

An apparatus and method for retorting oil shale using solar radiation. Oil shale is introduced into a first retorting chamber having a solar focus zone. There the oil shale is exposed to solar radiation and rapidly brought to a predetermined retorting temperature. Once the shale has reached this temperature, it is removed from the solar focus zone and transferred to a second retorting chamber where it is heated. In a second chamber, the oil shale is maintained at the retorting temperature, without direct exposure to solar radiation, until the retorting is complete.

Water mist injection in oil shale retorting

DOEpatents

Galloway, T.R.; Lyczkowski, R.W.; Burnham, A.K.

1980-07-30

Water mist is utilized to control the maximum temperature in an oil shale retort during processing. A mist of water droplets is generated and entrained in the combustion supporting gas flowing into the retort in order to distribute the liquid water droplets throughout the retort. The water droplets are vaporized in the retort in order to provide an efficient coolant for temperature control.

4. VIEW OF AREA EXCAVATED FOR ACCESS TO MERCURY RETORT. ...

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

4. VIEW OF AREA EXCAVATED FOR ACCESS TO MERCURY RETORT. VIEW SOUTH FROM RETORT. (OCTOBER, 1995) - McCormick Group Mine, Mercury Retort, East slope of Buckskin Mountain, Paradise Valley, Humboldt County, NV

Converting oil shale to liquid fuels: energy inputs and greenhouse gas emissions of the Shell in situ conversion process.

PubMed

Brandt, Adam R

2008-10-01

Oil shale is a sedimentary rock that contains kerogen, a fossil organic material. Kerogen can be heated to produce oil and gas (retorted). This has traditionally been a CO2-intensive process. In this paper, the Shell in situ conversion process (ICP), which is a novel method of retorting oil shale in place, is analyzed. The ICP utilizes electricity to heat the underground shale over a period of 2 years. Hydrocarbons are produced using conventional oil production techniques, leaving shale oil coke within the formation. The energy inputs and outputs from the ICP, as applied to oil shales of the Green River formation, are modeled. Using these energy inputs, the greenhouse gas (GHG) emissions from the ICP are calculated and are compared to emissions from conventional petroleum. Energy outputs (as refined liquid fuel) are 1.2-1.6 times greater than the total primary energy inputs to the process. In the absence of capturing CO2 generated from electricity produced to fuel the process, well-to-pump GHG emissions are in the range of 30.6-37.1 grams of carbon equivalent per megajoule of liquid fuel produced. These full-fuel-cycle emissions are 21%-47% larger than those from conventionally produced petroleum-based fuels.

Effects of retorting factors on combustion properties of shale char. 3. Distribution of residual organic matters.

PubMed

Han, Xiangxin; Jiang, Xiumin; Cui, Zhigang; Liu, Jianguo; Yan, Junwei

2010-03-15

Shale char, formed in retort furnaces of oil shale, is classified as a dangerous waste containing several toxic compounds. In order to retort oil shale to produce shale oil as well as treat shale char efficiently and in an environmentally friendly way, a novel kind of comprehensive utilization system was developed to use oil shale for shale oil production, electricity generation (shale char fired) and the extensive application of oil shale ash. For exploring the combustion properties of shale char further, in this paper organic matters within shale chars obtained under different retorting conditions were extracted and identified using a gas chromatography-mass spectrometry (GC-MS) method. Subsequently, the effects of retorting factors, including retorting temperature, residence time, particle size and heating rate, were analyzed in detail. As a result, a retorting condition with a retorting temperature of 460-490 degrees C, residence time of <40 min and a middle particle size was recommended for both keeping nitrogenous organic matters and aromatic hydrocarbons in shale char and improving the yield and quality of shale oil. In addition, shale char obtained under such retorting condition can also be treated efficiently using a circulating fluidized bed technology with fractional combustion. (c) 2009 Elsevier B.V. All rights reserved.

Laboratory study of the effects of combustion gases on retorting of Green River oil shale with superheated steam

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

Tyler, A.L.; Bullen, E.A.; Jacobs, H.R.

The leached zone of the Parachute Creek member of the Piceance Basin in the Green River Formation has a unique natural porosity that makes it a likely source for in-situ production of oil from oil shale by injection of superheated steam. The Equity Oil Co. of Salt Lake City, in cooperation with the U. S. Department of Energy, carried out field tests using surface generated steam. Difficulties in delivering steam of sufficiently high temperature to the formation resulted in an experiment which was only marginally successful yielding less than 1 percent of the estimated 300,000 barrels of oil in place.more » In 1981, personnel at Sandia National Laboratory suggested that a downhole steam generator which could produce steam at temperatures in excess of 1000/sup 0/F (538/sup 0/C) at depth could well solve the temperature problem. In order to evaluate the effects of combustion gases which would be injected along with steam, should a downhole steam generator be used, laboratory studies have been completed using steam diluted with CO/sub 2/ and with CO/sub 2/ and N/sub 2/ as the heating medium. Results of experiments in an autoclave reactor and in a laboratory retort are reported. The temperature, residence time, and partial pressure of steam are the parameters which effect oil yield and oil quality. Oil properties are reported for several experimental conditions and include oil yield, boiling point distributions, pour points, gravity, and elemental and hydrocarbon-type analyses. Both the autoclave and laboratory retort experiments indicate that CO/sub 2/ and N/sub 2/ do not take a reactive part in the formation of oils except as they dilute the steam. However, the presence of CO/sub 2/ in the gaseous atmosphere during retorting does promote a low-temperature transformation of dolomite to calcite in the inorganic matrix of the oil shale.« less

Bacterial physiological diversity in the rhizosphere of range plants in response to retorted shale stress. [Agropyron smithii Rydb; Atriplex canescens (Pursh) Nutt

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

Metzger, W.C.; Klein, D.A.; Redente, E.F.

1986-10-01

Bacterial populations were isolated from the soil-root interface and root-free regions of Agropyron smithii Rydb. and Atriplex canescens (Pursh) Nutt. grown in soil, retorted shale, or soil over shale. Bacteria isolated from retorted shale exhibited a wider range of tolerance to alkalinity and salinity and decreased growth on amino acid substrates compared with bacteria from soil and soil-over-shale environments. Exoenzyme production was only slightly affected by growth medium treatment. Viable bacterial populations were higher in the rhizosphere and rhizoplane of plants grown in retorted shale than in plants grown in soil or soil over shale. In addition, a greater numbermore » of physiological groups of rhizosphere bacteria was observed in retorted shale, compared with soil alone. Two patterns of community similarity were observed in comparisons of bacteria from soil over shale with those from soil and retorted-shale environments. Root-associated populations from soil over shale had a higher proportion of physiological groups in common with those from the soil control than those from the retorted-shale treatment. However, in non-rhizosphere populations, bacterial groups from soil over shale more closely resembled the physiological groups from retorted shale.« less

3. VIEW EAST OF TAILINGS OF MERCURY RETORT. SCOOP FOR ...

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

3. VIEW EAST OF TAILINGS OF MERCURY RETORT. SCOOP FOR EXTRACTING MERCURY VISIBLE IN CENTER OF PHOTOGRAPH. (OCTOBER, 1995) - McCormick Group Mine, Mercury Retort, East slope of Buckskin Mountain, Paradise Valley, Humboldt County, NV

EVALUATION OF THE EFFECTS OF WEATHERING ON A 50-YEAR OLD RETORTED OIL-SHALE WASTE PILE, RULISON EXPERIMENTAL RETORT, COLORADO.

USGS Publications Warehouse

Tuttle, Michele L.W.; Dean, Walter E.; Ackerman, Daniel J.; ,

1985-01-01

An oil-shale mine and experimental retort were operated near Rulison, Colorado by the U. S. Bureau of Mines from 1926 to 1929. Samples from seven drill cores from a retorted oil-shale waste pile were analyzed to determine 1) the chemical and mineral composition of the retorted oil shale and 2) variations in the composition that could be attributed to weathering. Unweathered, freshly-mined samples of oil shale from the Mahogany zone of the Green River Formation and slope wash collected away from the waste pile were also analyzed for comparison. The waste pile is composed of oil shale retorted under either low-temperature (400-500 degree C) or high-temperature (750 degree C) conditions. The results of the analyses show that the spent shale within the waste pile contains higher concentrations of most elements relative to unretorted oil shale.

RETORT ASSEMBLY

DOEpatents

Loomis, C.C.; Ash, W.J.

1957-11-26

An improved retort assembly useful in the thermal reduction of volatilizable metals such as magnesium and calcium is described. In this process a high vacuum is maintained in the retort, however the retort must be heated to very high temperatures while at the same time the unloading end must bo cooled to condense the metal vapors, therefore the retention of the vacuum is frequently difficult due to the thermal stresses involved. This apparatus provides an extended condenser sleeve enclosed by the retort cover which forms the vacuum seal. Therefore, the seal is cooled by the fluid in the condenser sleeve and the extreme thermal stresses found in previous designs together with the deterioration of the sealing gasket caused by the high temperatures are avoided.

Biological markers from Green River kerogen decomposition

NASA Astrophysics Data System (ADS)

Burnham, A. K.; Clarkson, J. E.; Singleton, M. F.; Wong, C. M.; Crawford, R. W.

1982-07-01

Isoprenoid and other carbon skeletons that are formed in living organisms and preserved essentially intact in ancient sediments are often called biological markers. The purpose of this paper is to develop improved methods of using isoprenoid hydrocarbons to relate petroleum or shale oil to its source rock. It is demonstrated that most, but not all, of the isoprenoid hydrocarbon structures are chemically bonded in kerogen (or to minerals) in Green River oil shale. The rate constant for thermally producing isoprenoid, cyclic, and aromatic hydrocarbons is substantially greater than for the bulk of shale oil. This may be related to the substantial quantity of CO 2 which is evolved coincident with the isoprenoid hydrocarbons but prior to substantial oil evolution. Although formation of isoprenoid alkenes is enhanced by rapid heating and high pyrolysis temperatures, the ratio of isoprenoid alkenes plus alkanes to normal alkenes plus alkanes is independent of heating rate. High-temperature laboratory pyrolysis experiments can thus be used to predict the distribution of aliphatic hydrocarbons in low temperature processes such as in situ shale oil production and perhaps petroleum formation. Finally, we demonstrate that significant variation in biological marker ratios occurs as a function of stratigraphy in the Green River formation. This information, combined with methods for measuring process yield from oil composition, enables one to relate time-dependent processing conditions to the corresponding time-dependent oil yield in a vertical modified- in situ retort even if there is a substantial and previously undetermined delay in drainage of shale oil from the retort.

The study of heat penetration of kimchi soup on stationary and rotary retorts.

PubMed

Cho, Won-Il; Park, Eun-Ji; Cheon, Hee Soon; Chung, Myong-Soo

2015-03-01

The aim of this study was to determine the heat-penetration characteristics using stationary and rotary retorts to manufacture Kimchi soup. Both heat-penetration tests and computer simulation based on mathematical modeling were performed. The sterility was measured at five different positions in the pouch. The results revealed only a small deviation of F 0 among the different positions, and the rate of heat transfer was increased by rotation of the retort. The thermal processing of retort-pouched Kimchi soup was analyzed mathematically using a finite-element model, and optimum models for predicting the time course of the temperature and F 0 were developed. The mathematical models could accurately predict the actual heat penetration of retort-pouched Kimchi soup. The average deviation of the temperature between the experimental and mathematical predicted model was 2.46% (R(2)=0.975). The changes in nodal temperature and F 0 caused by microbial inactivation in the finite-element model predicted using the NISA program were very similar to that of the experimental data of for the retorted Kimchi soup during sterilization with rotary retorts. The correlation coefficient between the simulation using the NISA program and the experimental data was very high, at 99%.

The Study of Heat Penetration of Kimchi Soup on Stationary and Rotary Retorts

PubMed Central

Cho, Won-Il; Park, Eun-Ji; Cheon, Hee Soon; Chung, Myong-Soo

2015-01-01

The aim of this study was to determine the heat-penetration characteristics using stationary and rotary retorts to manufacture Kimchi soup. Both heat-penetration tests and computer simulation based on mathematical modeling were performed. The sterility was measured at five different positions in the pouch. The results revealed only a small deviation of F0 among the different positions, and the rate of heat transfer was increased by rotation of the retort. The thermal processing of retort-pouched Kimchi soup was analyzed mathematically using a finite-element model, and optimum models for predicting the time course of the temperature and F0 were developed. The mathematical models could accurately predict the actual heat penetration of retort-pouched Kimchi soup. The average deviation of the temperature between the experimental and mathematical predicted model was 2.46% (R2=0.975). The changes in nodal temperature and F0 caused by microbial inactivation in the finite-element model predicted using the NISA program were very similar to that of the experimental data of for the retorted Kimchi soup during sterilization with rotary retorts. The correlation coefficient between the simulation using the NISA program and the experimental data was very high, at 99%. PMID:25866751

Study of the Use of Oxygen-Absorbing Packaging Material to Prolong Shelf-Life of Rations

DTIC Science & Technology

2010-05-28

technology can be used for retortable items (MRE 28 “Italian” entrée, chicken pesto with noodles ) since it maintained the 4 product shelf-life and...packages that have head spacing issues (e.g., retort item or those containing olive oil). Products included chicken pest with noodles (retorted entrée...of the MRE applesauce, they did not prevent the darkening problem. It is suspected that the retort processing step for applesauce manufacture may

Trace element partitioning during the retorting of Julia Creek oil shale

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

Patterson, J.H.; Dale, L.S.; Chapman, J.f.

1987-05-01

A bulk sample of oil shale from the Julia Creek deposit in Queensland was retorted under Fischer assay conditions at temperatures ranging from 250 to 550 /sup 0/C. The distributions of the trace elements detected in the shale oil and retort water were determined at each temperature. Oil distillation commenced at 300 /sup 0/C and was essentially complete at 500 /sup 0/C. A number of trace elements were progressively mobilized with increasing retort temperature up to 450 /sup 0/C. The following trace elements partitioned mainly to the oil: vanadium, arsenic, selenium, iron, nickel, titanium, copper, cobalt, and aluminum. Elements thatmore » also partitioned to the retort waters included arsenic, selenium, chlorine, and bromine. Element mobilization is considered to be caused by the volatilization of organometallic compounds, sulfide minerals, and sodium halides present in the oil shale. The results have important implications for shale oil refining and for the disposal of retort waters. 22 references, 5 tables.« less

Brazing retort manifold design concept may minimize air contamination and enhance uniform gas flow

NASA Technical Reports Server (NTRS)

Ruppe, E. P.

1966-01-01

Brazing retort manifold minimizes air contamination, prevents gas entrapment during purging, and provides uniform gas flow into the retort bell. The manifold is easily cleaned and turbulence within the bell is minimized because all manifold construction lies outside the main enclosure.

Method of operating an oil shale kiln

DOEpatents

Reeves, Adam A.

1978-05-23

Continuously determining the bulk density of raw and retorted oil shale, the specific gravity of the raw oil shale and the richness of the raw oil shale provides accurate means to control process variables of the retorting of oil shale, predicting oil production, determining mining strategy, and aids in controlling shale placement in the kiln for the retorting.

Leading trends in environmental regulation that affect energy development. Final report

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

Steele, R V; Attaway, L D; Christerson, J A

1980-01-01

Major environmental issues that are likely to affect the implementation of energy technologies between now and the year 2000 are identified and assessed. The energy technologies specifically addressed are: oil recovery and processing; gas recovery and processing; coal liquefaction; coal gasification (surface); in situ coal gasification; direct coal combustion; advanced power systems; magnetohydrodynamics; surface oil shale retorting; true and modified in situ oil shale retorting; geothermal energy; biomass energy conversion; and nuclear power (fission). Environmental analyses of these technologies included, in addition to the main processing steps, the complete fuel cycle from resource extraction to end use. A comprehensive surveymore » of the environmental community (including environmental groups, researchers, and regulatory agencies) was carried out in parallel with an analysis of the technologies to identify important future environmental issues. Each of the final 20 issues selected by the project staff has the following common attributes: consensus of the environmental community that the issue is important; it is a likely candidate for future regulatory action; it deals with a major environmental aspect of energy development. The analyses of the 20 major issues address their environmental problem areas, current regulatory status, and the impact of future regulations. These analyses are followed by a quantitative assessment of the impact on energy costs and nationwide pollutant emissions of possible future regulations. This is accomplished by employing the Strategic Environmental Assessment System (SEAS) for a subset of the 20 major issues. The report concludes with a more general discussion of the impact of environmental regulatory action on energy development.« less

Research continues on Julia Creek shale oil project

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

Not Available

1986-09-01

CSR Limited and the CSIRO Division of Mineral Engineering in Australia are working jointly on the development of a new retorting process for Julia Creek oil shale. This paper describes the retorting process which integrates a fluid bed combustor with a retort in which heat is transferred from hot shale ash to cold raw shale. The upgrading of shale oil into transport fuels is also described.

Desulfurized gas production from vertical kiln pyrolysis

DOEpatents

Harris, Harry A.; Jones, Jr., John B.

1978-05-30

A gas, formed as a product of a pyrolysis of oil shale, is passed through hot, retorted shale (containing at least partially decomposed calcium or magnesium carbonate) to essentially eliminate sulfur contaminants in the gas. Specifically, a single chambered pyrolysis vessel, having a pyrolysis zone and a retorted shale gas into the bottom of the retorted shale zone and cleaned product gas is withdrawn as hot product gas near the top of such zone.

Mercury isotope fractionation during ore retorting in the Almadén mining district, Spain

USGS Publications Warehouse

Gray, John E.; Pribil, Michael J.; Higueras, Pablo L.

2013-01-01

Almadén, Spain, is the world's largest mercury (Hg) mining district, which has produced over 250,000 metric tons of Hg representing about 30% of the historical Hg produced worldwide. The objective of this study was to measure Hg isotopic compositions of cinnabar ore, mine waste calcine (retorted ore), elemental Hg (Hg0(L)), and elemental Hg gas (Hg0(g)), to evaluate potential Hg isotopic fractionation. Almadén cinnabar ore δ202Hg varied from − 0.92 to 0.15‰ (mean of − 0.56‰, σ = 0.35‰, n = 7), whereas calcine was isotopically heavier and δ202Hg ranged from − 0.03‰ to 1.01‰ (mean of 0.43‰, σ = 0.44‰, n = 8). The average δ202Hg enrichment of 0.99‰ between cinnabar ore and calcines generated during ore retorting indicated Hg isotopic mass dependent fractionation (MDF). Mass independent fractionation (MIF) was not observed in any of the samples in this study. Laboratory retorting experiments of cinnabar also were carried out to evaluate Hg isotopic fractionation of products generated during retorting such as calcine, Hg0(L), and Hg0(g). Calcine and Hg0(L) generated during these retorting experiments showed an enrichment in δ202Hg of as much as 1.90‰ and 0.67‰, respectively, compared to the original cinnabar ore. The δ202Hg for Hg0(g) generated during the retorting experiments was as much as 1.16‰ isotopically lighter compared to cinnabar, thus, when cinnabar ore was roasted, the resultant calcines formed were isotopically heavier, whereas the Hg0(g) generated was isotopically lighter in Hg isotopes.

Review of samples of water, sediment, tailings, and biota at the Little Bonanza mercury mine, San Luis Obispo County, California

USGS Publications Warehouse

Rytuba, James J.; Hothem, Roger L.; Goldstein, Daniel N.; Brussee, Brianne E.; May, Jason T.

2011-01-01

Sample Sites and Methods Samples were collected to assess the concentrations of Hg and biogeochemically relevant constituents in tailings and wasterock piles at the Little Bonanza Hg mine. Tailings are present adjacent to a three-pipe retort used to process the Hg ore. The tailings occur in the upper 15 cm of the soil adjacent to the retort and slag from the retort is present on the surface. An area of disturbed soil and rock uphill from the retort was likely formed during construction of a dam that provided water for mining activities. Wasterock in these piles was sampled. The largest amount of tailings is exposed to the west of the retort in the bank of WF Las Tablas Creek. Water, sediment, and biota were sampled from WF Las Tablas Creek, which flows through the mine area. Sample-site locations are shown in figures 10 and 11 and listed in table 1. Samples were collected when streamflow was low and no precipitation had occurred.

Revegetation studies on Tosco II and USBM retorted oil shales

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

Kilkelly, M.K.; Harbert, H.P.; Berg, W.A.

1981-01-01

In 1973 studies on the revegetation of processed oil shales were initiated. The objectives of these studies were to investigate the vegetative stabilization of processed oil shales and to follow moisture and soluble salt movement in the retorted shale profile. Studies involving TOSCO II and USBM retorted shales were established at both a low-elevation (Anvil Points) and a high-elevation (Piceance Basin). Treatments included leaching and various depths of soil cover. After seven growing seasons a good vegetative cover remains with differences between treatments insignificant, with the exception of the TOSCO retorted shale south-aspect, which consistently supported less perennial vegetative covermore » than other treatments. With time, a shift from perennial grasses to dominance by shrubs was observed, especially on south-aspect slopes. 6 refs.« less

Apparatus for oil shale retorting

DOEpatents

Lewis, Arthur E.; Braun, Robert L.; Mallon, Richard G.; Walton, Otis R.

1986-01-01

A cascading bed retorting process and apparatus in which cold raw crushed shale enters at the middle of a retort column into a mixer stage where it is rapidly mixed with hot recycled shale and thereby heated to pyrolysis temperature. The heated mixture then passes through a pyrolyzer stage where it resides for a sufficient time for complete pyrolysis to occur. The spent shale from the pyrolyzer is recirculated through a burner stage where the residual char is burned to heat the shale which then enters the mixer stage.

Fuel Gas Demonstration Plant Program. Volume I. Demonstration plant

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

Not Available

1979-01-01

The objective of this project is for Babcock Contractors Inc. (BCI) to provide process designs, and gasifier retort design for a fuel gas demonstration plant for Erie Mining Company at Hoyt Lake, Minnesota. The fuel gas produced will be used to supplement natural gas and fuel oil for iron ore pellet induration. The fuel gas demonstration plant will consist of five stirred, two-stage fixed-bed gasifier retorts capable of handling caking and non-caking coals, and provisions for the installation of a sixth retort. The process and unit design has been based on operation with caking coals; however, the retorts have beenmore » designed for easy conversion to handle non-caking coals. The demonstration unit has been designed to provide for expansion to a commercial plant (described in Commercial Plant Package) in an economical manner.« less

Retort beef aroma that gives preferable properties to canned beef products and its aroma components.

PubMed

Migita, Koshiro; Iiduka, Takao; Tsukamoto, Kie; Sugiura, Sayuri; Tanaka, Genichiro; Sakamaki, Gousuke; Yamamoto, Yasufumi; Takeshige, Yusuke; Miyazawa, Toshio; Kojima, Ayako; Nakatake, Tomoko; Okitani, Akihiro; Matsuishi, Masanori

2017-12-01

The objective of this study is to identify the properties and responsible compounds for the aromatic roast odor (retort beef aroma) that commonly occurs in canned beef products and could contribute to their palatability. The optimal temperature for generating retort beef aroma was 121°C. An untrained panel evaluated both uncured corned beef and canned yamato-ni beef and found that they had an aroma that was significantly (P < 0.01) similar to the odor of 121°C-heated beef than 100°C-heated beef. The panel also noted that the aroma of 121°C-heated beef tended to be (P < 0.1) preferable than that of 100°C-heated beef. These results suggest that retort beef aroma is one constituent of palatability in canned beef. GC-MS (gas chromatography-mass spectrometry) analysis of the volatile fraction obtained from 100°C- and 121°C-heated beef showed that the amounts of pyrazine, 2-methylpyrazine and diacetyl were higher in the 121°C-heated beef than in the 100°C-heated beef. GC-sniffing revealed that the odor quality of pyrazines was similar to that of retort beef aroma. Therefore, pyrazines were suggested to be a candidate responsible for the retort beef aroma. Analysis of commercial uncured corned beef and cured corned beef confirmed the presence of pyrazine, 2-methylpyrazine and 2,6-dimethylpyrazine. © 2017 Japanese Society of Animal Science.

Feasibility of Applying Ohmic Heating and Split-Phase Aseptic Processing for Ration Entree Preservation

DTIC Science & Technology

1994-08-01

study demonstrated that either of these reduced- temperature sterilization processes will produce an acceptable product that is an alternative to thermal...and uniform heating of liquids and solids simultaneously, even of large particles, up to sterilization temperatures . Uniform heating means shorter...potential cost reduction by substitution of continuous processing of a high- temperature /short-time ( HTST ) nature for traditional batch retort

Overview of the Development of Australian Combat Ration Packs

DTIC Science & Technology

2014-12-01

g) Variety B Serve Size (g) Retort Meal Chilli Con Carne 1 x 250 FD Meal Veal Italienne 1 x 110 Instant Oriental Noodles 1 x 74 White Rice 2 x 125...retort pouch meal freeze dried meal flexible retort pouch meal light meals (soup, noodles , steak bar, canned fish)  noodles steak bar...Items Common to all HWRP Menus Cracked Pepper Vita Wheat 1x36 g instant coffee 1x3.5 g tea bags# 1x2.5 g cheddar cheese (canned) 1x56 g cappuccino

Integrated oil production and upgrading using molten alkali metal

DOEpatents

Gordon, John Howard

2016-10-04

A method that combines the oil retorting process (or other process needed to obtain/extract heavy oil or bitumen) with the process for upgrading these materials using sodium or other alkali metals. Specifically, the shale gas or other gases that are obtained from the retorting/extraction process may be introduced into the upgrading reactor and used to upgrade the oil feedstock. Also, the solid materials obtained from the reactor may be used as a fuel source, thereby providing the heat necessary for the retorting/extraction process. Other forms of integration are also disclosed.

Effect of combination processing on the microbial, chemical and sensory quality of ready-to-eat (RTE) vegetable pulav

NASA Astrophysics Data System (ADS)

Kumar, R.; George, Johnsy; Rajamanickam, R.; Nataraju, S.; Sabhapathy, S. N.; Bawa, A. S.

2011-12-01

Effect of irradiation in combination with retort processing on the shelf life and safety aspects of an ethnic Indian food product like vegetable pulav was investigated. Gamma irradiation of RTE vegetable pulav was carried out at different dosage rates with 60Co followed by retort processing. The combination processed samples were analysed for microbiological, chemical and sensory characteristics. Microbiological analysis indicated that irradiation in combination with retort processing has significantly reduced the microbial loads whereas the chemical and sensory analysis proved that this combination processing is effective in retaining the properties even after storage for one year at ambient conditions. The results also indicated that a minimum irradiation dosage at 4.0 kGy along with retort processing at an F0 value of 2.0 is needed to achieve the desired shelf life with improved organoleptic qualities.

Oil shale retorting and combustion system

DOEpatents

Pitrolo, Augustine A.; Mei, Joseph S.; Shang, Jerry Y.

1983-01-01

The present invention is directed to the extraction of energy values from l shale containing considerable concentrations of calcium carbonate in an efficient manner. The volatiles are separated from the oil shale in a retorting zone of a fluidized bed where the temperature and the concentration of oxygen are maintained at sufficiently low levels so that the volatiles are extracted from the oil shale with minimal combustion of the volatiles and with minimal calcination of the calcium carbonate. These gaseous volatiles and the calcium carbonate flow from the retorting zone into a freeboard combustion zone where the volatiles are burned in the presence of excess air. In this zone the calcination of the calcium carbonate occurs but at the expense of less BTU's than would be required by the calcination reaction in the event both the retorting and combustion steps took place simultaneously. The heat values in the products of combustion are satisfactorily recovered in a suitable heat exchange system.

Composition and Variation of Macronutrients, Immune Proteins, and Human Milk Oligosaccharides in Human Milk From Nonprofit and Commercial Milk Banks.

PubMed

Meredith-Dennis, Laura; Xu, Gege; Goonatilleke, Elisha; Lebrilla, Carlito B; Underwood, Mark A; Smilowitz, Jennifer T

2018-02-01

When human milk is unavailable, banked milk is recommended for feeding premature infants. Milk banks use processes to eliminate pathogens; however, variability among methods exists. Research aim: The aim of this study was to compare the macronutrient (protein, carbohydrate, fat, energy), immune-protective protein, and human milk oligosaccharide (HMO) content of human milk from three independent milk banks that use pasteurization (Holder vs. vat techniques) or retort sterilization. Randomly acquired human milk samples from three different milk banks ( n = 3 from each bank) were analyzed for macronutrient concentrations using a Fourier transform mid-infrared spectroscopy human milk analyzer. The concentrations of IgA, IgM, IgG, lactoferrin, lysozyme, α-lactalbumin, α antitrypsin, casein, and HMO were analyzed by mass spectrometry. The concentrations of protein and fat were significantly ( p < .05) less in the retort sterilized compared with the Holder and vat pasteurized samples, respectively. The concentrations of all immune-modulating proteins were significantly ( p < .05) less in the retort sterilized samples compared with vat and/or Holder pasteurized samples. The total HMO concentration and HMOs containing fucose, sialic acid, and nonfucosylated neutral sugars were significantly ( p < .05) less in retort sterilized compared with Holder pasteurized samples. Random milk samples that had undergone retort sterilization had significantly less immune-protective proteins and total and specific HMOs compared with samples that had undergone Holder and vat pasteurization. These data suggest that further analysis of the effect of retort sterilization on human milk components is needed prior to widespread adoption of this process.

Process for oil shale retorting using gravity-driven solids flow and solid-solid heat exchange

DOEpatents

Lewis, A.E.; Braun, R.L.; Mallon, R.G.; Walton, O.R.

1983-09-21

A cascading bed retorting process and apparatus are disclosed in which cold raw crushed shale enters at the middle of a retort column into a mixer stage where it is rapidly mixed with hot recycled shale and thereby heated to pyrolysis temperature. The heated mixture then passes through a pyrolyzer stage where it resides for a sufficient time for complete pyrolysis to occur. The spent shale from the pyrolyzer is recirculated through a burner stage where the residual char is burned to heat the shale which then enters the mixer stage.

Process for oil shale retorting using gravity-driven solids flow and solid-solid heat exchange

DOEpatents

Lewis, Arthur E.; Braun, Robert L.; Mallon, Richard G.; Walton, Otis R.

1986-01-01

A cascading bed retorting process and apparatus in which cold raw crushed shale enters at the middle of a retort column into a mixer stage where it is rapidly mixed with hot recycled shale and thereby heated to pyrolysis temperature. The heated mixture then passes through a pyrolyzer stage where it resides for a sufficient time for complete pyrolysis to occur. The spent shale from the pyrolyzer is recirculated through a burner stage where the residual char is burned to heat the shale which then enters the mixer stage.

Effect of retorted-oil shale leachate on a blue-green alga (Anabaena flos-aquae)

USGS Publications Warehouse

McKnight, Diane M.; Pereira, Wilfred E.; Rostad, Colleen E.; Stiles, Eric A.

1983-01-01

In the event of the development of the large oil shale reserves of Colorado, Utah, and Wyoming, one of the main environmental concerns will be disposal of retorted-oil shale which will be generated in greater volume than the original volume oI the mined oil shale. Investigators have found that leachates of retorted-oil shale are alkaline and have large concentrations of dissolved solids, molybdenum, boron, and fluoride (STOLLENWERK & RUNNELS 1981). STOLLENWERK & RUNNELS (1981) concluded that drainage from waste shale piles could have deleterious effects on the water quality of streams in northwestern Colorado.

System for utilizing oil shale fines

DOEpatents

Harak, Arnold E.

1982-01-01

A system is provided for utilizing fines of carbonaceous materials such as particles or pieces of oil shale of about one-half inch or less diameter which are rejected for use in some conventional or prior surface retorting process, which obtains maximum utilization of the energy content of the fines and which produces a waste which is relatively inert and of a size to facilitate disposal. The system includes a cyclone retort (20) which pyrolyzes the fines in the presence of heated gaseous combustion products, the cyclone retort having a first outlet (30) through which vapors can exit that can be cooled to provide oil, and having a second outlet (32) through which spent shale fines are removed. A burner (36) connected to the spent shale outlet of the cyclone retort, burns the spent shale with air, to provide hot combustion products (24) that are carried back to the cyclone retort to supply gaseous combustion products utilized therein. The burner heats the spent shale to a temperature which forms a molten slag, and the molten slag is removed from the burner into a quencher (48) that suddenly cools the molten slag to form granules that are relatively inert and of a size that is convenient to handle for disposal in the ground or in industrial processes.

Talaromyces sayulitensis, Acidiella bohemica and Penicillium citrinum in Brazilian oil shale by-products.

PubMed

de Goes, Kelly C G P; da Silva, Josué J; Lovato, Gisele M; Iamanaka, Beatriz T; Massi, Fernanda P; Andrade, Diva S

2017-12-01

Fine shale particles and retorted shale are waste products generated during the oil shale retorting process. These by-products are small fragments of mined shale rock, are high in silicon and also contain organic matter, micronutrients, hydrocarbons and other elements. The aims of this study were to isolate and to evaluate fungal diversity present in fine shale particles and retorted shale samples collected at the Schist Industrialization Business Unit (Six)-Petrobras in São Mateus do Sul, State of Paraná, Brazil. Combining morphology and internal transcribed spacer (ITS) sequence, a total of seven fungal genera were identified, including Acidiella, Aspergillus, Cladosporium, Ochroconis, Penicillium, Talaromyces and Trichoderma. Acidiella was the most predominant genus found in the samples of fine shale particles, which are a highly acidic substrate (pH 2.4-3.6), while Talaromyces was the main genus in retorted shale (pH 5.20-6.20). Talaromyces sayulitensis was the species most frequently found in retorted shale, and Acidiella bohemica in fine shale particles. The presence of T. sayulitensis, T. diversus and T. stolli in oil shale is described herein for the first time. In conclusion, we have described for the first time a snapshot of the diversity of filamentous fungi colonizing solid oil shale by-products from the Irati Formation in Brazil.

Explosively produced fracture of oil shale

NASA Astrophysics Data System (ADS)

Morris, W. A.

1982-05-01

Rock fragmentation research in oil shale to develop the blasting technologies and designs required to prepare a rubble bed for a modified in situ retort is reported. Experimental work is outlined, proposed studies in explosive characterization are detailed and progress in numerical calculation techniques to predict fracture of the shale is described. A detailed geologic characterization of two Anvil Points experiment sites is related to previous work at Colony Mine. The second section focuses on computer modeling and theory. The latest generation of the stress wave code SHALE, its three dimensional potential, and the slide line package for it are described. A general stress rate equation that takes energy dependence into account is discussed.

21 CFR 113.3 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-04-01

... steam into the closed retort and the time when the retort reaches the required processing temperature..., school, penal, or other organization) processing of food, including pet food. Persons engaged in the... flames to achieve sterilization temperatures. A holding period in a heated section may follow the initial...

Innovative food processing technology using ohmic heating and aseptic packaging for meat.

PubMed

Ito, Ruri; Fukuoka, Mika; Hamada-Sato, Naoko

2014-02-01

Since the Tohoku earthquake, there is much interest in processed foods, which can be stored for long periods at room temperature. Retort heating is one of the main technologies employed for producing it. We developed the innovative food processing technology, which supersede retort, using ohmic heating and aseptic packaging. Electrical heating involves the application of alternating voltage to food. Compared with retort heating, which uses a heat transfer medium, ohmic heating allows for high heating efficiency and rapid heating. In this paper we ohmically heated chicken breast samples and conducted various tests on the heated samples. The measurement results of water content, IMP, and glutamic acid suggest that the quality of the ohmically heated samples was similar or superior to that of the retort-heated samples. Furthermore, based on the monitoring of these samples, it was observed that sample quality did not deteriorate during storage. © 2013. Published by Elsevier Ltd on behalf of The American Meat Science Association. All rights reserved.

Lethality of Rendang packaged in multilayer retortable pouch with sterilization process

NASA Astrophysics Data System (ADS)

Praharasti, A. S.; Kusumaningrum, A.; Frediansyah, A.; Nurhikmat, A.; Khasanah, Y.; Suprapedi

2017-01-01

Retort Pouch had become a choice to preserve foods nowadays, besides the used of the can. Both had their own advantages, and Retort Pouch became more popular for the reason of cheaper and easier to recycle. General Method usually used to estimate the lethality of commercial heat sterilization process. Lethality value wa s used for evaluating the efficacy of the thermal process. This study aimed to find whether different layers of pouch materials affect the lethality value and to find differences lethality in two types of multilayer retort pouch, PET/Aluminum Foil/Nylon/RCPP and PET/Nylon/Modified Aluminum/CPP. The result showed that the different layer arrangement was resulted different Sterilization Value (SV). PET/Nylon/Modified Aluminum/CPP had better heat penetration, implied by the higher value of lethality. PET/Nylon/Modified Aluminum/CPP had the lethality value of 6,24 minutes, whereas the lethality value of PET/Aluminum Foil/Nylon/RCPP was 3,54 minutes.

Combined fluidized bed retort and combustor

DOEpatents

Shang, Jer-Yu; Notestein, John E.; Mei, Joseph S.; Zeng, Li-Wen

1984-01-01

The present invention is directed to a combined fluidized bed retorting and combustion system particularly useful for extracting energy values from oil shale. The oil-shale retort and combustor are disposed side-by-side and in registry with one another through passageways in a partition therebetween. The passageways in the partition are submerged below the top of the respective fluid beds to preclude admixing or the product gases from the two chambers. The solid oil shale or bed material is transported through the chambers by inclining or slanting the fluidizing medium distributor so that the solid bed material, when fluidized, moves in the direction of the downward slope of the distributor.

A new laboratory approach to shale analysis using NMR relaxometry

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.; Baez, Luis; Beeney, Ken; Sonnenberg, Steve

2013-01-01

Low-field nuclear magnetic resonance (LF-NMR) relaxometry is a non-invasive technique commonly used to assess hydrogen-bearing fluids in petroleum reservoir rocks. Measurements made using LF-NMR provide information on rock porosity, pore-size distributions, and in some cases, fluid types and saturations (Timur, 1967; Kenyon et al., 1986; Straley et al., 1994; Brown, 2001; Jackson, 2001; Kleinberg, 2001; Hurlimann et al., 2002). Recent improvements in LF-NMR instrument electronics have made it possible to apply methods used to measure pore fluids to assess highly viscous and even solid organic phases within reservoir rocks. T1 and T2 relaxation responses behave very differently in solids and liquids; therefore the relationship between these two modes of relaxation can be used to differentiate organic phases in rock samples or to characterize extracted organic materials. Using T1-T2 correlation data, organic components present in shales, such as kerogen and bitumen, can be examined in laboratory relaxometry measurements. In addition, implementation of a solid-echo pulse sequence to refocus T2 relaxation caused by homonuclear dipolar coupling during correlation measurements allows for improved resolution of solid-phase protons. LF-NMR measurements of T1 and T2 relaxation time distributions were carried out on raw oil shale samples from the Eocene Green River Formation and pyrolyzed samples of these shales processed by hydrous pyrolysis and techniques meant to mimic surface and in-situ retorting. Samples processed using the In Situ Simulator approach ranged from bitumen and early oil generation through to depletion of petroleum generating potential. The standard T1-T2 correlation plots revealed distinct peaks representative of solid- and liquid-like organic phases; results on the pyrolyzed shales reflect changes that occurred during thermal processing. The solid-echo T1 and T2 measurements were used to improve assessment of the solid organic phases, specifically kerogen, thermally degraded kerogen, and char. Integrated peak areas from the LF-NMR results representative of kerogen and bitumen were found to be well correlated with S1 and S2 parameters from Rock-Eval programmed pyrolysis. This study demonstrates that LFNMR relaxometry can provide a wide range of information on shales and other reservoir rocks that goes well beyond porosity and pore-fluid analysis.

Four dimensional X-ray imaging of deformation modes in organic-rich Green River Shale retorted under uniaxial compression

NASA Astrophysics Data System (ADS)

Kobchenko, M.; Pluymakers, A.; Cordonnier, B.; Tairova, A.; Renard, F.

2017-12-01

Time-lapse imaging of fracture network development in organic-rich shales at elevated temperatures while kerogen is retorted allows characterizing the development of microfractures and the onset of primary migration. When the solid organic matter is transformed to hydrocarbons with lower molecular weight, the local pore-pressure increases and drives the propagation of hydro-fractures sub-parallel to the shale lamination. On the scale of samples of several mm size, these fractures can be described as mode I opening, where fracture walls dilate in the direction of minimal compression. However, so far experiments coupled to microtomography in situ imaging have been performed on samples where no load was imposed. Here, an external load was applied perpendicular to the sample laminations and we show that this stress state slows down, but does not stop, the propagation of fracture along bedding. Conversely, microfractures also propagate sub-perpendicular to the shale lamination, creating a percolating network in three dimensions. To monitor this process we have used a uniaxial compaction rig combined with in-situ heating from 50 to 500 deg C, while capturing three-dimensional X-ray microtomography scans at a voxel resolution of 2.2 μm; Data were acquired at beamline ID19 at the European Synchrotron Radiation Facility. In total ten time-resolved experiments were performed at different vertical loading conditions, with and without lateral passive confinement and different heating rates. At high external load the sample fails by symmetric bulging, while at lower external load the reaction-induced fracture network develops with the presence of microfractures both sub-parallel and sub-perpendicular to the bedding direction. In addition, the variation of experimental conditions allows the decoupling of the effects of the hydrocarbon decomposition reaction on the deformation process from the influence of thermal stress heating on the weakening and failure mode of immature shale.

FIELD STUDIES ON USBM AND TOSCO II RETORTED OIL SHALES: VEGETATION, MOISTURE, SALINITY, AND RUNOFF, 1977-1980

EPA Science Inventory

Field studies were initiated in 1973 to investigate the vegetative stabilization of processed oil shales and to follow moisture and soluble salt movement within the soil/shale profile. Research plots with two types of retorted shales (TOSCO II and USBM) with leaching and soil cov...

120. VIEW, LOOKING SOUTHEAST, OF TELLURIDE IRON WORKS RETORT USED ...

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

120. VIEW, LOOKING SOUTHEAST, OF TELLURIDE IRON WORKS RETORT USED FOR FLASHING MERCURY OFF OF GOLD TO CREATE SOFT INGOTS CALLED "SPONGES." AT RIGHT ARE SAFES FOR STORING 22-POUND SPONGES WORTH OVER $60,000 EACH, CA. 1985. - Shenandoah-Dives Mill, 135 County Road 2, Silverton, San Juan County, CO

Yield and Production Properties of Wood chips and Particles Torrefied in a Crucible Furnace Retort

Treesearch

Thomas L. Eberhardt; Chi-Leung So; Karen G. Reed

2016-01-01

Biomass preprocessing by torrefaction improves feedstock consistency and thereby improves the efficiency of biofuels operations, including pyrolysis, gasification, and combustion. A crucible furnace retort was fabricated of sufficient size to handle a commercially available wood chip feedstock. Varying the torrefaction times and temperatures provided an array of...

1. Distant view shows Engine Room Building behind cranes. Retort ...

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

1. Distant view shows Engine Room Building behind cranes. Retort rings in foreground were once located in Engine Room Building. See photo WA-131-A-2. Building on left is Machine Shop. Boiler Building is in front of stack. - Pacific Creosoting Plant, Engine Room Building, 5350 Creosote Place, Northeast, Bremerton, Kitsap County, WA

9 CFR 318.308 - Deviations in processing.

Code of Federal Regulations, 2011 CFR

2011-01-01

...) Deviations in processing (or process deviations) must be handled according to: (1)(i) A HACCP plan for canned..., containers in the retort intake valve and in transfer valves between retort shells at the time of a jam or... 9 Animals and Animal Products 2 2011-01-01 2011-01-01 false Deviations in processing. 318.308...

9 CFR 381.308 - Deviations in processing.

Code of Federal Regulations, 2011 CFR

2011-01-01

..., containers in the retort intake valve and in transfer valves between retort shells at the time of a jam or... 9 Animals and Animal Products 2 2011-01-01 2011-01-01 false Deviations in processing. 381.308... Deviations in processing. (a) Whenever the actual process is less than the process schedule or when any...

40 CFR Appendix 7 to Subpart A of... - API Recommended Practice 13B-2

Code of Federal Regulations, 2010 CFR

2010-07-01

... facilitate cleaning and funnel-shaped top to catch falling drops. For compliance monitoring under the NPDES... condenser. b. Pack the retort body with steel wool. c. Apply lubricant/sealant to threads of retort cup and... the clean and dry liquid receiver. This is mass (C), grams. Place the receiver below condenser outlet...

40 CFR Appendix 7 to Subpart A of... - API Recommended Practice 13B-2

Code of Federal Regulations, 2011 CFR

2011-07-01

... facilitate cleaning and funnel-shaped top to catch falling drops. For compliance monitoring under the NPDES... condenser. b. Pack the retort body with steel wool. c. Apply lubricant/sealant to threads of retort cup and... the clean and dry liquid receiver. This is mass (C), grams. Place the receiver below condenser outlet...

Technical note: Evaluation of a crucible furnace retort for laboratory torrefactions of wood chips

Treesearch

Thomas L. Eberhardt; Karen G. Reed

2014-01-01

Torrefaction is a thermal process that improves biomass performance as a fuel by property enhancements such as decreased moisture uptake and increased carbon density. Most studies to date have used very small amounts of finely ground biomass. This study reports the testing of a crucible furnace retort that was fabricated to produce intermediate quantities of torrefied...

Shale-oil-recovery systems incorporating ore beneficiation. Final report.

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

Weiss, M.A.; Klumpar, I.V.; Peterson, C.R.

This study analyzed the recovery of oil from oil shale by use of proposed systems which incorporate beneficiation of the shale ore (that is concentration of the kerogen before the oil-recovery step). The objective was to identify systems which could be more attractive than conventional surface retorting of ore. No experimental work was carried out. The systems analyzed consisted of beneficiation methods which could increase kerogen concentrations by at least four-fold. Potentially attractive low-enrichment methods such as density separation were not examined. The technical alternatives considered were bounded by the secondary crusher as input and raw shale oil as output.more » A sequence of ball milling, froth flotation, and retorting concentrate is not attractive for Western shales compared to conventional ore retorting; transporting the concentrate to another location for retorting reduces air emissions in the ore region but cost reduction is questionable. The high capital and energy cost s results largely from the ball milling step which is very inefficient. Major improvements in comminution seem achievable through research and such improvements, plus confirmation of other assumptions, could make high-enrichment beneficiation competitive with conventional processing. 27 figures, 23 tables.« less

Optimization of thermal processing of canned mussels.

PubMed

Ansorena, M R; Salvadori, V O

2011-10-01

The design and optimization of thermal processing of solid-liquid food mixtures, such as canned mussels, requires the knowledge of the thermal history at the slowest heating point. In general, this point does not coincide with the geometrical center of the can, and the results show that it is located along the axial axis at a height that depends on the brine content. In this study, a mathematical model for the prediction of the temperature at this point was developed using the discrete transfer function approach. Transfer function coefficients were experimentally obtained, and prediction equations fitted to consider other can dimensions and sampling interval. This model was coupled with an optimization routine in order to search for different retort temperature profiles to maximize a quality index. Both constant retort temperature (CRT) and variable retort temperature (VRT; discrete step-wise and exponential) were considered. In the CRT process, the optimal retort temperature was always between 134 °C and 137 °C, and high values of thiamine retention were achieved. A significant improvement in surface quality index was obtained for optimal VRT profiles compared to optimal CRT. The optimization procedure shown in this study produces results that justify its utilization in the industry.

Shale oil recovery process

DOEpatents

Zerga, Daniel P.

1980-01-01

A process of producing within a subterranean oil shale deposit a retort chamber containing permeable fragmented material wherein a series of explosive charges are emplaced in the deposit in a particular configuration comprising an initiating round which functions to produce an upward flexure of the overburden and to initiate fragmentation of the oil shale within the area of the retort chamber to be formed, the initiating round being followed in a predetermined time sequence by retreating lines of emplaced charges developing further fragmentation within the retort zone and continued lateral upward flexure of the overburden. The initiating round is characterized by a plurality of 5-spot patterns and the retreating lines of charges are positioned and fired along zigzag lines generally forming retreating rows of W's. Particular time delays in the firing of successive charges are disclosed.

Molecular characterization and comparison of shale oils generated by different pyrolysis methods using FT-ICR mass spectrometry

USGS Publications Warehouse

Jin, J.M.; Kim, S.; Birdwell, J.E.

2011-01-01

Fourier transform ion cyclotron resonance mass spectrometry (FT ICR-MS) was applied in the analysis of shale oils generated using two different pyrolysis systems under laboratory conditions meant to simulate surface and in situ oil shale retorting. Significant variations were observed in the shale oils, particularly the degree of conjugation of the constituent molecules. Comparison of FT ICR-MS results to standard oil characterization methods (API gravity, SARA fractionation, gas chromatography-flame ionization detection) indicated correspondence between the average Double Bond Equivalence (DBE) and asphaltene content. The results show that, based on the average DBE values and DBE distributions of the shale oils examined, highly conjugated species are enriched in samples produced under low pressure, high temperature conditions and in the presence of water.

WATER COOLED RETORT COVER

DOEpatents

Ash, W.J.; Pozzi, J.F.

1962-05-01

A retort cover is designed for use in the production of magnesium metal by the condensation of vaporized metal on a collecting surface. The cover includes a condensing surface, insulating means adjacent to the condensing surface, ind a water-cooled means for the insulating means. The irrangement of insulation and the cooling means permits the magnesium to be condensed at a high temperature and in massive nonpyrophoric form. (AEC)

Quality of ready to serve tilapia fish curry with PUFA in retortable pouches.

PubMed

Dhanapal, K; Reddy, G V S; Nayak, B B; Basu, S; Shashidhar, K; Venkateshwarlu, G; Chouksey, M K

2010-09-01

Studies on the physical, chemical, and microbiological qualities of fresh tilapia meat revealed its suitability for the preparation of ready to eat fish curry packed in retort pouches. Studies on the fatty acid profile of tilapia meat suggest fortification with polyunsaturated fatty acid (PUFA) to increase the nutritional value. Based on the commercial sterility, sensory evaluation, color, and texture profile analysis F(0) value of 6.94 and cook value of 107.24, with a total process time of 50.24 min at 116 °C was satisfactory for the development of tilapia fish curry in retort pouches. Thermally processed ready to eat south Indian type tilapia fish curry fortified with PUFA was developed and its keeping quality studied at ambient temperature. During storage, a slight increase in the fat content of fish meat was observed, with no significant change in the contents of moisture, protein, and ash. The thiobarbituric acid (TBA) values of fish curry significantly increased during storage. Fish curry fortified with 1% cod liver oil and fish curry without fortification (control) did not show any significant difference in the levels of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), during thermal processing and storage. Sensory analysis revealed that fortification of fish curry with cod liver oil had no impact on the quality. Tilapia fish curry processed at 116 °C and F(0) value of 7.0 (with or without fortification of cod liver oil) was fit for consumption, even after a period of 1-y storage in retort pouch. Tilapia is a lean variety of fish with white flesh and therefore an ideal choice as raw material for the development of ready to serve fish products such as fish curry in retort pouches for both domestic and international markets. Ready to eat thermal processed (116 °C and F(0) value of 7.0) south Indian type tilapia fish curry enriched with PUFA and packed in retort pouch was acceptable for consumption even after a storage period of 1 y at ambient temperature.

Assessment of the long-term stability of retort pouch foods to support extended duration spaceflight.

PubMed

Catauro, Patricia M; Perchonok, Michele H

2012-01-01

To determine the suitability of retort processed foods to support long-duration spaceflight, a series of 36-mo accelerated shelf life studies were performed on 13 representative retort pouch products. Combined sensory evaluations, physical properties assessments, and nutritional analyses were employed to determine shelf life endpoints for these foods, which were either observed during the analysis or extrapolated via mathematical projection. Data obtained through analysis of these 13 products were later used to estimate the shelf life values of all retort-processed spaceflight foods. In general, the major determinants of shelf life appear to be the development of off-flavor and off-color in products over time. These changes were assumed to be the result of Maillard and oxidation reactions, which can be initiated or accelerated as a result of the retort process and product formulation. Meat products and other vegetable entrées are projected to maintain their quality the longest, between 2 and 8 y, without refrigeration. Fruit and dessert products (1.5 to 5 y), dairy products (2.5 to 3.25 y), and starches, vegetable, and soup products (1 to 4 y) follow. Aside from considerable losses in B and C vitamin content, nutritional value of most products was maintained throughout shelf life. Fortification of storage-labile vitamins was proposed as a countermeasure to ensure long-term nutritive value of these products. The use of nonthermal sterilization technologies was also recommended, as a means to improve initial quality of these products and extend their shelf life for use in long-duration missions. Data obtained also emphasize the importance of low temperature storage in maintaining product quality. Retort sterilized pouch products are garnering increased commercial acceptance, largely due to their improved convenience and quality over metal-canned products. Assessment of the long-term stability of these products with ambient storage can identify potential areas for improvement, and ultimately increase consumer satisfaction with these technologies. Journal of Food Science © 2011 Institute of Food Technologists® No claim to original US government works.

Effect of high pressure-high temperature process on meat product quality

NASA Astrophysics Data System (ADS)

Duranton, Frédérique; Marée, Elvire; Simonin, Hélène; Chéret, Romuald; de Lamballerie, Marie

2011-03-01

High pressure/high temperature (HPHT) processing is an innovative way to sterilize food and has been proposed as an alternative to conventional retorting. By using elevated temperatures and adiabatic compression, it allows the inactivation of vegetative microorganisms and pathogen spores. Even though the microbial inactivation has been widely studied, the effect of such process on sensorial attributes of food products, especially meat products, remains rare. The aim of this study was to investigate the potential of using HPHT process (500 MPa/115 °C) instead of conventional retorting to stabilize Toulouse sausages while retaining high organoleptic quality. The measurements of texture, color, water-holding capacity and microbial stability were investigated. It was possible to manufacture stable products at 500 MPa/115 °C/30 min. However, in these conditions, no improvement of the quality was found compared with conventional retorting.

Method of design for vertical oil shale retorting vessels and retorting therewith

DOEpatents

Reeves, Adam A.

1978-01-03

A method of designing the gas flow parameters of a vertical shaft oil shale retorting vessel involves determining the proportion of gas introduced in the bottom of the vessel and into intermediate levels in the vessel to provide for lateral distribution of gas across the vessel cross section, providing mixing with the uprising gas, and determining the limiting velocity of the gas through each nozzle. The total quantity of gas necessary for oil shale treatment in the vessel may be determined and the proportion to be injected into each level is then determined based on the velocity relation of the orifice velocity and its feeder manifold gas velocity. A limitation is placed on the velocity of gas issuing from an orifice by the nature of the solid being treated, usually physical tests of gas velocity impinging the solid.

Process for oil shale retorting

DOEpatents

Jones, John B.; Kunchal, S. Kumar

1981-10-27

Particulate oil shale is subjected to a pyrolysis with a hot, non-oxygenous gas in a pyrolysis vessel, with the products of the pyrolysis of the shale contained kerogen being withdrawn as an entrained mist of shale oil droplets in a gas for a separation of the liquid from the gas. Hot retorted shale withdrawn from the pyrolysis vessel is treated in a separate container with an oxygenous gas so as to provide combustion of residual carbon retained on the shale, producing a high temperature gas for the production of some steam and for heating the non-oxygenous gas used in the oil shale retorting process in the first vessel. The net energy recovery includes essentially complete recovery of the organic hydrocarbon material in the oil shale as a liquid shale oil, a high BTU gas, and high temperature steam.

Mercury reduction in Munhena, Mozambique: homemade solutions and the social context for change.

PubMed

Spiegel, Samuel J; Savornin, Olivier; Shoko, Dennis; Veiga, Marcello M

2006-01-01

The health and environmental impacts of artisanal gold mining are of growing concern in Munhena, Mozambique, where more than 12,000 people are involved in such activities. Gold is extracted using mercury amalgamation, posing a considerable threat to human and environmental health. A pilot project ascertained the feasibility of reducing mercury use and emissions by promoting control measures utilizing local resources. Retorts were fabricated with local materials. Training workshops introduced the homemade retorts, and a portable mercury monitor revealed effective mercury reduction. Barriers to widespread technology adoption include poverty, lack of knowledge and trust, and the free supply of mercury from private gold buyers. Homemade retorts are inexpensive and effective, and miners could benefit by building community amalgamation centers. The government could play a greater role in gold purchasing to reduce mercury pollution.

Geotechnical Properties of Oil Shale Retorted by the PARAHO and TOSCO Processes.

DTIC Science & Technology

1979-11-01

literature search was restricted to the Green River formation of oil shale in the tri-state area of Colorado (Piceance Basin ), Utah ( Uinta Basin ), and...it is preheated by combustion gases as it travels downward by gravity. Air and recycling gas are injected at midheight and are burned, bringing the oil ...REFERENCES..................................38 TABLES 1-5 APPENDIX A: OIL SHALE RETORTING PROCESSES................Al Tosco Process Gas Combustion

Retortable Laminate/Polymeric Food Tubes for Specialized Feeding

DTIC Science & Technology

2012-06-01

on commercial off-the-shelf materials and not military unique. A market survey of commercially available laminated tubes revealed that they are all...on commercial off-the-shelf materials and not military unique. A market survey of commercially available laminated tubes revealed that they are...available materials and not be uniquely military. We surveyed the market for laminated retortable tubes and were not able to find any application

Oil shale combustor model developed by Greek researchers

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

Not Available

1986-09-01

Work carried out in the Department of Chemical Engineering at the University of Thessaloniki, Thessaloniki, Greece has resulted in a model for the combustion of retorted oil shale in a fluidized bed combustor. The model is generally applicable to any hot-solids retorting process, whereby raw oil shale is retorted by mixing with a hot solids stream (usually combusted spent shale), and then the residual carbon is burned off the spent shale in a fluidized bed. Based on their modelling work, the following conclusions were drawn by the researchers. (1) For the retorted particle size distribution selected (average particle diameter 1600more » microns) complete carbon conversion is feasible at high pressures (2.7 atmosphere) and over the entire temperature range studied (894 to 978 K). (2) Bubble size was found to have an important effect, especially at conditions where reaction rates are high (high temperature and pressure). (3) Carbonate decomposition increases with combustor temperature and residence time. Complete carbon conversion is feasible at high pressures (2.7 atmosphere) with less than 20 percent carbonate decomposition. (4) At the preferred combustor operating conditions (high pressure, low temperature) the main reaction is dolomite decomposition while calcite decomposition is negligible. (5) Recombination of CO/sub 2/ with MgO occurs at low temperatures, high pressures, and long particle residence times.« less

Reduction of Aspergillus spp. and aflatoxins in peanut sauce processing by oil-less frying of chilli powder and retort processing.

PubMed

Farawahida, A H; Jinap, S; Nor-Khaizura, M A R; Samsudin, N I P

2017-12-01

Among the many roles played by small and medium enterprises (SMEs) in the food industry is the production of heritage foods such as peanut sauce. Unfortunately, the safety of peanut sauce is not always assured as the processing line is not controlled. Peanut sauce is usually made of peanuts and chilli, and these commodities are normally contaminated with Aspergillus spp. and aflatoxins (AFs). Hence, the objective of this study was to evaluate the practices related to reduction of AF hazard and the effect of interventions in peanut sauce processing. Peanut samples were collected from each step of peanut sauce processing from a small peanut sauce company according to four designs: (1) control; (2) oil-less frying of chilli powder; (3) addition of retort processing; and (4) combination of oil-less frying of chilli powder and retort processing. Oil-less frying of chilli powder (Design 2) reduced total AFs by 33-41%, retort processing (Design 3) reduced total AFs by 49%, while combination of these two thermal processes (Design 4) significantly reduced total AFs, by 57%. The present work demonstrated that Design 4 yielded the highest reduction of total AFs and is therefore recommended to be employed by SME companies.

Oil shale retort apparatus

DOEpatents

Reeves, Adam A.; Mast, Earl L.; Greaves, Melvin J.

1990-01-01

A retorting apparatus including a vertical kiln and a plurality of tubes for delivering rock to the top of the kiln and removal of processed rock from the bottom of the kiln so that the rock descends through the kiln as a moving bed. Distributors are provided for delivering gas to the kiln to effect heating of the rock and to disturb the rock particles during their descent. The distributors are constructed and disposed to deliver gas uniformly to the kiln and to withstand and overcome adverse conditions resulting from heat and from the descending rock. The rock delivery tubes are geometrically sized, spaced and positioned so as to deliver the shale uniformly into the kiln and form symmetrically disposed generally vertical paths, or "rock chimneys", through the descending shale which offer least resistance to upward flow of gas. When retorting oil shale, a delineated collection chamber near the top of the kiln collects gas and entrained oil mist rising through the kiln.

Influence of irrigation and weathering reactions on the composition of percolates from retorted oil shale in field lysimeters

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

Garland, T. R.; Wildung, R. E.; Harbert, H. P.

1979-04-01

Major cations, anions, trace elements and dissolved organic C were measured in percolate from retorted oil shale collected from irrigated lysimeters in the field at Anvil Points, Colorado, over a two year period. The investigations indicated that chemical equilibrium was not established over the monitoring period and major changes occurred in percolate composition as a function of applied water volume and water residence time in the shale. Field and laboratory studies indicated that several factors contributed to changes in the chemistry of the shale on weathering, including recarbonization of the surface horizons with atmospheric CO/sub 2/ and the activities ofmore » microorganisms in surface and subsurface horizons. However, the principal mechanism responsible for the decreases in pH and salt concentrations appeared to be the conversion of major quantities of sulfide in the retorted shale to sulfate through a thiosulfate intermediate.« less

Field studies on USBM and TOSCO II retorted oil shales: vegetation, moisture, salinity, and runoff, 1977-1980. Final report

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

Kilkelly, M.K.; Berg, W.A.; Harbert, H.P. III

1981-08-01

Field studies were initiated in 1973 to investigate the vegetative stabilization of processed oil shales and to follow moisture and soluble salt movement within the soil/shale profile. Research plots with two types of retorted shales (TOSCO II and USBM) with leaching and soil cover treatments were established at two locations: low-elevation (Anvil Points) and high-elevation (Piceance Basin) in western Colorado. Vegetation was established by intensive management including leaching, N and P fertilization, seeding, mulching, and irrigation. After seven growing seasons, a good vegetative cover remained with few differences between treatments, with the exception of the TOSCO retorted shale, south-aspect, whichmore » consistently supported less perennial vegetative cover than other treatments. With time, a shift from perennial grasses to dominance by shrubs was observed. Rodent activity on some treatments had a significantly negative effect on vegetative cover.« less

Process concept of retorting of Julia Creek oil shale

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

Sitnai, O.

1984-06-01

A process is proposed for the above ground retorting of the Julia Creek oil shale in Queensland. The oil shale characteristics, process description, chemical reactions of the oil shale components, and the effects of variable and operating conditions on process performance are discussed. The process contains a fluidized bed combustor which performs both as a combustor of the spent shales and as a heat carrier generator for the pyrolysis step. 12 references, 5 figures, 5 tables.

Collected Works of Mao Tse-Tung (1917-1949), Volume 4

DTIC Science & Technology

1978-10-10

Spanking of children had not been com- pletely stopped, but it was reduced. (There should be no spanking at all.) The children had become more...intelligent. In the past, when spanked or scolded by their parents, they seldom retorted, but now more of them re- torted. (If the parents did not... spank or scold them, the children would not be retorting.) About 1 percent of the women married 3 times in the 4-1/2 years after the uprising

Geology and phosphate resources of the Hawley Creek area, Lemhi County, Idaho

USGS Publications Warehouse

Oberlindacher, Peter; Hovland, Robert David

1979-01-01

Phosphate resources occur within the Retort Phosphatic Shale Member of the Permian Phosphoria Formation in the Hawley Creek area, near Leadore, in east-central Idaho. About 12 square miles (31 km2 ) of the Retort Member and enclosing rocks were mapped at a scale of 1:12,000 to evaluate the leasable Federal mineral resources. The Retort has an average thickness of 73 feet (22.3 m) and 12.9 linear miles (20.8 linear km) of outcrop within the area mapped. Rock samples taken from a bulldozer trench were analyzed for phosphate content and for minor trace elements. Analyses show a cumulative thickness of 8.7 feet ( 2.7 m) of medium-grade phosphate rock ( 24 to 31 percent P2O5) and 33.4 feet (10.2 m) of low-grade phosphate rock (16 to 24 percent P2O5). Minor elements in the Retort include uranium, vanadium, fluorine, cadmium, chromium, nickel, molybdenum, silver, and rare earths. These minor elements are potential byproducts of any future phosphate production in the Hawley Creek area. In addition, analyses of six phosphate rock samples taken from a prospect trench show a cumulative thickness of 14.9 ft (4.5 m) at 17.6 percent P2O5. Indicated phosphate resources are calculated for phosphate beds under less than 600 feet (183.0 m) of overburden. Approximately 36.5 feet (11.1 m), representing 50 percent of the total Retort Member, were measured in trench CP-71. There are 80.42 million short tons (72.96 million metric tons) of medium-grade phosphate rock, and 308.76 million short tons ( 280.10 million metric tons) of low-grade phosphate rock in the Retort Member within the map area. Because the thickness and grade of the phosphate beds for each block are based on the recovered section from CP-71, the calculated phosphate resource estimates represent a minimum. Other mineral resources in the area are thorium (35 ppm) in a Precambrian (?) granite body located immediately west of the Hawley Creek area; oil and gas accumulations may occur beneath the Medicine Lodge thrust system in this part of the Beaverhead Mountains. Paleozoic, Mesozoic, and Cenozoic rocks are present in the Hawley Creek area. Fold axes and thrust faults have a dominant northwest trend. These thrusts and folds are probably associated with the northeast-oriented stress field that existed in Late Cretaceous time. Evidence of younger, high-angle normal and reverse faults in the area also exists.

Combuston method of oil shale retorting

DOEpatents

Jones, Jr., John B.; Reeves, Adam A.

1977-08-16

A gravity flow, vertical bed of crushed oil shale having a two level injection of air and a three level injection of non-oxygenous gas and an internal combustion of at least residual carbon on the retorted shale. The injection of air and gas is carefully controlled in relation to the mass flow rate of the shale to control the temperature of pyrolysis zone, producing a maximum conversion of the organic content of the shale to a liquid shale oil. The parameters of the operation provides an economical and highly efficient shale oil production.

Staged fluidized bed

DOEpatents

Mallon, R.G.

1983-05-13

The invention relates to oil shale retorting and more particularly to staged fluidized bed oil shale retorting. Method and apparatus are disclosed for narrowing the distribution of residence times of any size particle and equalizing the residence times of large and small particles in fluidized beds. Particles are moved up one fluidized column and down a second fluidized column with the relative heights selected to equalize residence times of large and small particles. Additional pairs of columns are staged to narrow the distribution of residence times and provide complete processing of the material.

Improved mechanical properties of retorted carrots by ultrasonic pre-treatments.

PubMed

Day, Li; Xu, Mi; Øiseth, Sofia K; Mawson, Raymond

2012-05-01

The use of ultrasound pre-processing treatment, compared to blanching, to enhance mechanical properties of non-starchy cell wall materials was investigated using carrot as an example. The mechanical properties of carrot tissues were measured by compression and tensile testing after the pre-processing treatment prior to and after retorting. Carrot samples ultrasound treated for 10 min at 60 °C provided a higher mechanical strength (P<0.05) to the cell wall structure than blanching for the same time period. With the addition of 0.5% CaCl(2) in the pre-treatment solution, both blanching and ultrasound treatment showed synergistic effect on enhancing the mechanical properties of retorted carrot pieces. At a relatively short treatment time (10 min at 60 °C) with the use of 0.5% CaCl(2), ultrasound treatment achieved similar enhancement to the mechanical strength of retorted carrots to blanching for a much longer time period (i.e. 40 min). The mechanism involved appears to be related to the stress responses present in all living plant matter. However, there is a need to clarify the relative importance of the potential stress mechanisms in order to get a better understanding of the processing conditions likely to be most effective. The amount of ultrasound treatment required is likely to involve low treatment intensities and there are indications from the structural characterisation and mechanical property analyses that the plant cell wall tissues were more elastic than that accomplished using low temperature long time blanching. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

High-pressure thermal sterilization: food safety and food quality of baby food puree.

PubMed

Sevenich, Robert; Kleinstueck, Elke; Crews, Colin; Anderson, Warwick; Pye, Celine; Riddellova, Katerina; Hradecky, Jaromir; Moravcova, Eliska; Reineke, Kai; Knorr, Dietrich

2014-02-01

The benefits that high-pressure thermal sterilization offers as an emerging technology could be used to produce a better overall food quality. Due to shorter dwell times and lower thermal load applied to the product in comparison to the thermal retorting, lower numbers and quantities of unwanted food processing contaminants (FPCs), for example, furan, acrylamide, HMF, and MCPD-esters could be formed. Two spore strains were used to test the technique; Geobacillus stearothermophilus and Bacillus amyloliquefaciens, over the temperature range 90 to 121 °C at 600 MPa. The treatments were carried out in baby food puree and ACES-buffer. The treatments at 90 and 105 °C showed that G. stearothermophilus is more pressure-sensitive than B. amyloliquefaciens. The formation of FPCs was monitored during the sterilization process and compared to the amounts found in retorted samples of the same food. The amounts of furan could be reduced between 81% to 96% in comparison to retorting for the tested temperature pressure combination even at sterilization conditions of F₀-value in 7 min. © 2014 Institute of Food Technologists®

Effect of γ-irradiation on commercial polypropylene based mono and multi-layered retortable food packaging materials

NASA Astrophysics Data System (ADS)

George, Johnsy; Kumar, R.; Sajeevkumar, V. A.; Sabapathy, S. N.; Vaijapurkar, S. G.; Kumar, D.; Kchawahha, A.; Bawa, A. S.

2007-07-01

Irradiation processing of food in the prepackaged form may affect chemical and physical properties of the plastic packaging materials. The effect of γ-irradiation doses (2.5-10.0 kGy) on polypropylene (PP)-based retortable food packaging materials, were investigated using Fourier transform infrared (FTIR) spectroscopic analysis, which revealed the changes happening to these materials after irradiation. The mechanical properties decreased with irradiation while oxygen transmission rate (OTR) was not affected significantly. Colour measurement indicated that Nylon 6 containing multilayer films became yellowish after irradiation. Thermal characterization revealed the changes in percentage crystallinity.

Plowshare Program - American Atomic Bomb Tests For Industrial Applications

ScienceCinema

None

2018-01-16

The United States Atomic Energy Commission (AEC) established the Plowshare Program as a research and development activity to explore the technical and economic feasibility of using nuclear explosives for industrial applications. The reasoning was that the relatively inexpensive energy available from nuclear explosions could prove useful for a wide variety of peaceful purposes. The Plowshare Program began in 1958 and continued through 1975. Between December 1961 and May 1973, the United States conducted 27 Plowshare nuclear explosive tests comprising 35 individual detonations. Conceptually, industrial applications resulting from the use of nuclear explosives could be divided into two broad categories: 1) large-scale excavation and quarrying, where the energy from the explosion was used to break up and/or move rock; and 2) underground engineering, where the energy released from deeply buried nuclear explosives increased the permeability and porosity of the rock by massive breaking and fracturing. Possible excavation applications included: canals, harbors, highway and railroad cuts through mountains, open pit mining, construction of dams, and other quarry and construction-related projects. Underground nuclear explosion applications included: stimulation of natural gas production, preparation of leachable ore bodies for in situ leaching, creation of underground zones of fractured oil shale for in situ retorting, and formation of underground natural gas and petroleum storage reservoirs.

Plowshare Program - American Atomic Bomb Tests For Industrial Applications

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

None

2012-04-22

The United States Atomic Energy Commission (AEC) established the Plowshare Program as a research and development activity to explore the technical and economic feasibility of using nuclear explosives for industrial applications. The reasoning was that the relatively inexpensive energy available from nuclear explosions could prove useful for a wide variety of peaceful purposes. The Plowshare Program began in 1958 and continued through 1975. Between December 1961 and May 1973, the United States conducted 27 Plowshare nuclear explosive tests comprising 35 individual detonations. Conceptually, industrial applications resulting from the use of nuclear explosives could be divided into two broad categories: 1)more » large-scale excavation and quarrying, where the energy from the explosion was used to break up and/or move rock; and 2) underground engineering, where the energy released from deeply buried nuclear explosives increased the permeability and porosity of the rock by massive breaking and fracturing. Possible excavation applications included: canals, harbors, highway and railroad cuts through mountains, open pit mining, construction of dams, and other quarry and construction-related projects. Underground nuclear explosion applications included: stimulation of natural gas production, preparation of leachable ore bodies for in situ leaching, creation of underground zones of fractured oil shale for in situ retorting, and formation of underground natural gas and petroleum storage reservoirs.« less

Bacteria and Bioactivity in Holder Pasteurized and Shelf-Stable Human Milk Products

PubMed Central

2017-01-01

Abstract Background: Historically, Holder pasteurization has been used to pasteurize donor human milk available in a hospital setting. There is extensive research that provides an overview of the impact of Holder pasteurization on bioactive components of human milk. A shelf-stable (SS) human milk product, created using retort processing, recently became available; however, to our knowledge, little has been published about the effect of retort processing on human milk. Objective: We aimed to assess the ability of retort processing to eliminate bacteria and to quantify the difference in lysozyme and secretory immunoglobulin A (sIgA) activity between Holder pasteurized (HP) and SS human milk. Methods: Milk samples from 60 mothers were pooled. From this pool, 36 samples were taken: 12 samples were kept raw, 12 samples were HP, and 12 samples were retort processed to create an SS product. All samples were analyzed for total aerobic bacteria, coliform bacteria, Bacillus cereus, sIgA activity, and lysozyme activity. Raw samples served as the control. Results: One raw sample and 3 HP samples contained B. cereus at the time of culture. There were no detectable bacteria in SS samples at the time of culture. Raw samples had significantly greater lysozyme and sIgA activity than HP and SS samples (P < 0.0001). HP samples retained significantly more lysozyme and sIgA activity (54% and 87%, respectively) than SS samples (0% and 11%, respectively). Conclusions: Human milk processed using Holder pasteurization should continue to be screened for the presence of B. cereus. Clinicians should be aware of the differences in the retention of lysozyme and sIgA activity in HP and SS products when making feeding decisions for medically fragile or immunocompromised infants to ensure that patients are receiving the maximum immune protection. PMID:29955718

Paraho environmental data. Part I. Process characterization. Par II. Air quality. Part III. Water quality

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

Heistand, R.N.; Atwood, R.A.; Richardson, K.L.

1980-06-01

From 1973 to 1978, Development Engineering, Inc. (DEI), a subsidiary of Paraho Development Corporation, demostrated the Paraho technology for surface oil shale retorting at Anvil Points, Colorado. A considerable amount of environmentally-related research was also conducted. This body of data represents the most comprehensive environmental data base relating to surface retorting that is currently available. In order to make this information available, the DOE Office of Environment has undertaken to compile, assemble, and publish this environmental data. The compilation has been prepared by DEI. This report includes the process characterization, air quality, and water quality categories.

Double Retort System for Materials Compatibility Testing

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

V. Munne; EV Carelli

2006-02-23

With Naval Reactors (NR) approval of the Naval Reactors Prime Contractor Team (NRPCT) recommendation to develop a gas cooled reactor directly coupled to a Brayton power conversion system as the Space Nuclear Power Plant (SNPP) for Project Prometheus (References a and b) there was a need to investigate compatibility between the various materials to be used throughout the SNPP. Of particular interest was the transport of interstitial impurities from the nickel-base superalloys, which were leading candidates for most of the piping and turbine components to the refractory metal alloys planned for use in the reactor core. This kind of contaminationmore » has the potential to affect the lifetime of the core materials. This letter provides technical information regarding the assembly and operation of a double retort materials compatibility testing system and initial experimental results. The use of a double retort system to test materials compatibility through the transfer of impurities from a source to a sink material is described here. The system has independent temperature control for both materials and is far less complex than closed loops. The system is described in detail and the results of three experiments are presented.« less

Israeli co-retorting of coal and oil shale would break even at 22/barrel

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

Not Available

Work is being carried out at the Hebrew University of Jerusalem on co-retorting of coal and oil shale. The work is funded under a cooperative agreement with the US Department of Energy. The project is exploring the conversion of US eastern high-sulfur bituminous coal in a split-stage, fluidized-bed reactor. Pyrolysis occurs in the first stage and char combustion in the second stage. These data for coal will be compared with similar data from the same reactor fueled by high-sulfur eastern US oil shale and Israeli oil shales. The project includes research at three major levels: pyrolysis in lab-scale fluidized-bed reactor;more » retorting in split-stage, fluidized-bed bench-scale process (1/4 tpd); and scale-up, preparation of full-size flowchart, and economic evaluation. In the past year's research, a preliminary economic evaluation was completed for a scaled-up process using a feed of high-sulfur coal and carbonate-containing Israeli oil shale. A full-scale plant in Israel was estimated to break even at an equivalent crude oil price of $150/ton ($22/barrel).« less

Downhole delay assembly for blasting with series delay

DOEpatents

Ricketts, Thomas E.

1982-01-01

A downhole delay assembly is provided which can be placed into a blasthole for initiation of explosive in the blasthole. The downhole delay assembly includes at least two detonating time delay devices in series in order to effect a time delay of longer than about 200 milliseconds in a round of explosions. The downhole delay assembly provides a protective housing to prevent detonation of explosive in the blasthole in response to the detonation of the first detonating time delay device. There is further provided a connection between the first and second time delay devices. The connection is responsive to the detonation of the first detonating time delay device and initiates the second detonating time delay device. A plurality of such downhole delay assemblies are placed downhole in unfragmented formation and are initiated simultaneously for providing a round of explosive expansions. The explosive expansions can be used to form an in situ oil shale retort containing a fragmented permeable mass of formation particles.

Analysis of the effectiveness of steam retorting of oil shale

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

Jacobs, H.R.; Pensel, R.W.; Udell, K.S.

A numerical model is developed to describe the retorting of oil shale using superheated steam. The model describes not only the temperature history of the shale but predicts the evolution of shale oil from kerogen decomposition and the breakdown of the carbonates existing in the shale matrix. The heat transfer coefficients between the water and the shale are determined from experiments utilizing the model to reduce the data. Similarly the model is used with thermogravimetric analysis experiments to develop an improved kinetics expression for kerogen decomposition in a steam environment. Numerical results are presented which indicate the effect of oilmore » shale particle size and steam temperature on oil production.« less

Method for retorting oil shale

DOEpatents

Shang, Jer-Yu; Lui, A.P.

1985-08-16

The recovery of oil from oil shale is provided in a fluidized bed by using a fluidizing medium of a binary mixture of carbon dioxide and 5 steam. The mixture with a steam concentration in the range of about 20 to 75 volume percent steam provides an increase in oil yield over that achievable by using a fluidizing gas of carbon dioxide or steam alone when the mixture contains higher steam concentrations. The operating parameters for the fluidized bed retorted are essentially the same as those utilized with other gaseous fluidizing mediums with the significant gain being in the oil yield recovered which is attributable solely to the use of the binary mixture of carbon dioxide and steam. 2 figs.

Meals for the Elderly

NASA Technical Reports Server (NTRS)

1980-01-01

The aim of Skylab's multi-agency cooperative project was to make simple but nutritious space meals available to handicapped and otherwise homebound senior adults, unable to take advantage of existing meal programs sponsored by federal, state and private organizations. As a spinoff of Meal Systems for the Elderly, commercial food processing firms are now producing astronaut type meals for public distribution. Company offers variety of freeze dried foods which are reconstituted by addition of water, and "retort pouch" meals which need no reconstitution, only heating. The retort pouch is an innovative flexible package that combines the advantage of boil-in bag and metal can. Foods retain their flavor, minerals and vitamins can be stored without refrigeration and are lightweight for easy transportation.

Commercially sterilized mussel meats (Mytilus chilensis): a study on process yield.

PubMed

Almonacid, S; Bustamante, J; Simpson, R; Urtubia, A; Pinto, M; Teixeira, A

2012-06-01

The processing steps most responsible for yield loss in the manufacture of canned mussel meats are the thermal treatments of precooking to remove meats from shells, and thermal processing (retorting) to render the final canned product commercially sterile for long-term shelf stability. The objective of this study was to investigate and evaluate the impact of different combinations of process variables on the ultimate drained weight in the final mussel product (Mytilu chilensis), while verifying that any differences found were statistically and economically significant. The process variables selected for this study were precooking time, brine salt concentration, and retort temperature. Results indicated 2 combinations of process variables producing the widest difference in final drained weight, designated best combination and worst combination with 35% and 29% yield, respectively. Significance of this difference was determined by employing a Bootstrap methodology, which assumes an empirical distribution of statistical error. A difference of nearly 6 percentage points in total yield was found. This represents a 20% increase in annual sales from the same quantity of raw material, in addition to increase in yield, the conditions for the best process included a retort process time 65% shorter than that for the worst process, this difference in yield could have significant economic impact, important to the mussel canning industry. © 2012 Institute of Food Technologists®

Spatial and stratigraphic distribution of water in oil shale of the Green River Formation using Fischer Assay, Piceance Basin, northwestern Colorado

USGS Publications Warehouse

Johnson, Ronald C.; Mercier, Tracey J.; Brownfield, Michael E.

2014-01-01

The spatial and stratigraphic distribution of water in oil shale of the Eocene Green River Formation in the Piceance Basin of northwestern Colorado was studied in detail using some 321,000 Fischer assay analyses in the U.S. Geological Survey oil-shale database. The oil-shale section was subdivided into 17 roughly time-stratigraphic intervals, and the distribution of water in each interval was assessed separately. This study was conducted in part to determine whether water produced during retorting of oil shale could provide a significant amount of the water needed for an oil-shale industry. Recent estimates of water requirements vary from 1 to 10 barrels of water per barrel of oil produced, depending on the type of retort process used. Sources of water in Green River oil shale include (1) free water within clay minerals; (2) water from the hydrated minerals nahcolite (NaHCO3), dawsonite (NaAl(OH)2CO3), and analcime (NaAlSi2O6.H20); and (3) minor water produced from the breakdown of organic matter in oil shale during retorting. The amounts represented by each of these sources vary both stratigraphically and areally within the basin. Clay is the most important source of water in the lower part of the oil-shale interval and in many basin-margin areas. Nahcolite and dawsonite are the dominant sources of water in the oil-shale and saline-mineral depocenter, and analcime is important in the upper part of the formation. Organic matter does not appear to be a major source of water. The ratio of water to oil generated with retorting is significantly less than 1:1 for most areas of the basin and for most stratigraphic intervals; thus water within oil shale can provide only a fraction of the water needed for an oil-shale industry.

Spatial and stratigraphic distribution of water in oil shale of the Green River Formation using Fischer assay, Piceance Basin, northwestern Colorado

USGS Publications Warehouse

Johnson, Ronald C.; Mercier, Tracey J.; Brownfield, Michael E.

2014-01-01

The spatial and stratigraphic distribution of water in oil shale of the Eocene Green River Formation in the Piceance Basin of northwestern Colorado was studied in detail using some 321,000 Fischer assay analyses in the U.S. Geological Survey oil-shale database. The oil-shale section was subdivided into 17 roughly time-stratigraphic intervals, and the distribution of water in each interval was assessed separately. This study was conducted in part to determine whether water produced during retorting of oil shale could provide a significant amount of the water needed for an oil-shale industry. Recent estimates of water requirements vary from 1 to 10 barrels of water per barrel of oil produced, depending on the type of retort process used. Sources of water in Green River oil shale include (1) free water within clay minerals; (2) water from the hydrated minerals nahcolite (NaHCO3), dawsonite (NaAl(OH)2CO3), and analcime (NaAlSi2O6.H20); and (3) minor water produced from the breakdown of organic matter in oil shale during retorting. The amounts represented by each of these sources vary both stratigraphically and areally within the basin. Clay is the most important source of water in the lower part of the oil-shale interval and in many basin-margin areas. Nahcolite and dawsonite are the dominant sources of water in the oil-shale and saline-mineral depocenter, and analcime is important in the upper part of the formation. Organic matter does not appear to be a major source of water. The ratio of water to oil generated with retorting is significantly less than 1:1 for most areas of the basin and for most stratigraphic intervals; thus water within oil shale can provide only a fraction of the water needed for an oil-shale industry.

A Transversely Isotropic Thermo-mechanical Framework for Oil Shale

NASA Astrophysics Data System (ADS)

Semnani, S. J.; White, J. A.; Borja, R. I.

2014-12-01

The present study provides a thermo-mechanical framework for modeling the temperature dependent behavior of oil shale. As a result of heating, oil shale undergoes phase transformations, during which organic matter is converted to petroleum products, e.g. light oil, heavy oil, bitumen, and coke. The change in the constituents and microstructure of shale at high temperatures dramatically alters its mechanical behavior e.g. plastic deformations and strength, as demonstrated by triaxial tests conducted at multiple temperatures [1,2]. Accordingly, the present model formulates the effects of changes in the chemical constituents due to thermal loading. It is well known that due to the layered structure of shale its mechanical properties in the direction parallel to the bedding planes is significantly different from its properties in the perpendicular direction. Although isotropic models simplify the modeling process, they fail to accurately describe the mechanical behavior of these rocks. Therefore, many researchers have studied the anisotropic behavior of rocks, including shale [3]. The current study presents a framework to incorporate the effects of transverse isotropy within a thermo-mechanical formulation. The proposed constitutive model can be readily applied to existing finite element codes to predict the behavior of oil shale in applications such as in-situ retorting process and stability assessment in petroleum reservoirs. [1] Masri, M. et al."Experimental Study of the Thermomechanical Behavior of the Petroleum Reservoir." SPE Eastern Regional/AAPG Eastern Section Joint Meeting. Society of Petroleum Engineers, 2008. [2] Xu, B. et al. "Thermal impact on shale deformation/failure behaviors---laboratory studies." 45th US Rock Mechanics/Geomechanics Symposium. American Rock Mechanics Association, 2011. [3] Crook, AJL et al. "Development of an orthotropic 3D elastoplastic material model for shale." SPE/ISRM Rock Mechanics Conference. Society of Petroleum Engineers, 2002.

Isotopic Variability of Mercury in Ore, Mine-Waste Calcine, and Leachates of Mine-Waste Calcine from Areas Mined for Mercury

PubMed Central

2009-01-01

The isotopic composition of mercury (Hg) was determined in cinnabar ore, mine-waste calcine (retorted ore), and leachates obtained from water leaching experiments of calcine from two large Hg mining districts in the U.S. This study is the first to report significant mass-dependent Hg isotopic fractionation between cinnabar ore and resultant calcine. Data indicate that δ202Hg values relative to NIST 3133 of calcine (up to 1.52‰) in the Terlingua district, Texas, are as much as 3.24‰ heavier than cinnabar (−1.72‰) prior to retorting. In addition, δ202Hg values obtained from leachates of Terlingua district calcines are isotopically similar to, or as much as 1.17‰ heavier than associated calcines, most likely due to leaching of soluble, byproduct Hg compounds formed during ore retorting that are a minor component in the calcines. As a result of the large fractionation found between cinnabar and calcine, and because calcine is the dominant source of Hg contamination from the mines studied, δ202Hg values of calcine may be more environmentally important in these mined areas than the primary cinnabar ore. Measurement of the Hg isotopic composition of calcine is necessary when using Hg isotopes for tracing Hg sources from areas mined for Hg, especially mine water runoff. PMID:19848142

Isotopic variability of mercury in ore, mine-waste calcine, and leachates of mine-waste calcine from areas mined for mercury

USGS Publications Warehouse

Stetson, S.J.; Gray, J.E.; Wanty, R.B.; Macalady, D.L.

2009-01-01

The isotopic composition of mercury (Hg) was determined in cinnabar ore, mine-waste calcine (retorted ore), and leachates obtained from water leaching experiments of calcine from two large Hg mining districts in the U.S. This study is the first to report significant mass-dependent Hg isotopic fractionation between cinnabar ore and resultant calcine. Data indicate that ??202Hg values relative to NIST 3133 of calcine (up to 1.52???) in the Terlingua district, Texas, are as much as 3.24??? heavier than cinnabar (-1.72???) prior to retorting. In addition, ??202Hg values obtained from leachates of Terlingua district calcines are isotopically similar to, or as much as 1.17??? heavier than associated calcines, most likely due to leaching of soluble, byproduct Hg compounds formed during ore retorting that are a minor component in the calcines. As a result of the large fractionation found between cinnabar and calcine, and because calcine is the dominant source of Hg contamination from the mines studied, ??202Hg values of calcine may be more environmentally important in these mined areas than the primary cinnabar ore. Measurement of the Hg isotopic composition of calcine is necessary when using Hg isotopes for tracing Hg sources from areas mined for Hg, especially mine water runoff. ?? 2009 American Chemical Society.

Hydrocarbon recovery from diatomite

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

Scinta, J.

1984-05-15

Supercritical extraction of diatomaceous earth results in a much more significant improvement in hydrocarbon recovery over Fischer retorting than achievable with tar sands. Process and apparatus for supercritical extraction of diatomaceous earth are disclosed.

SPOUTED BED DESIGN CONSIDERATIONS FOR COATED NUCLEAR FUEL PARTICLES

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

Marshall, Douglas W.

High Temperature Gas Cooled Reactors (HTGRs) are fueled with tristructural isotropic (TRISO) coated nuclear fuel particles embedded in a carbon-graphite fuel body. TRISO coatings consist of four layers of pyrolytic carbon and silicon carbide that are deposited on uranium ceramic fuel kernels (350µm – 500µm diameters) in a concatenated series of batch depositions. Each layer has dedicated functions such that the finished fuel particle has its own integral containment to minimize and control the release of fission products into the fuel body and reactor core. The TRISO coatings are the primary containment structure in the HTGR reactor and must havemore » very high uniformity and integrity. To ensure high quality TRISO coatings, the four layers are deposited by chemical vapor deposition (CVD) using high purity precursors and are applied in a concatenated succession of batch operations before the finished product is unloaded from the coating furnace. These depositions take place at temperatures ranging from 1230°C to 1550°C and use three different gas compositions, while the fuel particle diameters double, their density drops from 11.1 g/cm3 to 3.0 g/cm3, and the bed volume increases more than 8-fold. All this is accomplished without the aid of sight ports or internal instrumentation that could cause chemical contamination within the layers or mechanical damage to thin layers in the early stages of each layer deposition. The converging section of the furnace retort was specifically designed to prevent bed stagnation that would lead to unacceptably high defect fractions and facilitate bed circulation to avoid large variability in coating layer dimensions and properties. The gas injection nozzle was designed to protect precursor gases from becoming overheated prior to injection, to induce bed spouting and preclude bed stagnation in the bottom of the retort. Furthermore, the retort and injection nozzle designs minimize buildup of pyrocarbon and silicon carbide on the retort wall and manage nozzle orifice accretions. The equipment and operating methods have yielded very good reproducibility in the TRISO coated particles batches.« less

In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

DOE PAGES

Liu, Y.; Wang, H.; Zhang, X.

2015-11-30

Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentationmore » studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.« less

Rehabilitation potential and practices of Colorado oil shale lands. Progress report, June 1, 1978--May 31, 1979

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

Cook, C.W.

The following document is a third-year progress report for the period June 1, 1978 to May 31, 1979. The overall objective of the project is to study the effects of seeding techniques, species mixtures, fertilizer, ecotypes, improved plant materials, mycorrhizal fungi, and soil microorganisms on the initial and final stages of reclamation obtained through seeding and subsequent succession on disturbed oil shale lands. Plant growth medias that are being used in field-established test plots include retorted shale, soil over retorted shale, subsoil materials, and surface disturbed topsoils. Because of the long-term nature of successional and ecologically oriented studies the projectmore » is just beginning to generate significant publications. Several of the studies associated with the project have some phases being conducted principally in the laboratories and greenhouses at Colorado State Univerisity. The majority of the research, however, is being conducted on a 20 hectare Intensive Study Site located near the focal points of oil shale activity in the Piceance Basin. The site is at an elevation of 2,042 m, receives approximately 30 to 55 cm of precipitation annually, and encompasses the plant communities most typical of the Piceance Basin. Most of the information contained in this report originated from the monitoring and sampling of research plots established in either the fall of 1976 or 1977. Therefore, data that have been obtained from the Intensive Study Site represent only first- or second-year results. However, many trends have been identified in thesuccessional process and the soil microorganisms and mycorrhizal studies continue to contribute significant information to the overall results. The phytosociological study has progressed to a point where field sampling is complete and the application and publication of this materials will be forthcoming in 1979.« less

Method and apparatus for hydrocarbon recovery from tar sands

DOEpatents

Westhoff, J.D.; Harak, A.E.

1988-05-04

A method and apparatus for utilizing tar sands having a broad range of bitumen content is disclosed. More particularly, tar sands are pyrolyzed in a cyclone retort with high temperature gases recycled from the cyclone retort to produce oil and hydrocarbon products. The spent tar sands are then burned at 2000/degree/F in a burner to remove residual char and produce a solid waste that is easily disposable. The process and apparatus have the advantages of being able to utilize tar sands having a broad range of bitumen content and the advantage of producing product gases that are free from combustion gases and thereby have a higher heating value. Another important advantage is rapid pyrolysis of the tar sands in the cyclone so as to effectively utilize smaller sized reactor vessels for reducing capitol and operating costs. 1 fig., 1 tab.

Solar heated oil shale pyrolysis process

NASA Technical Reports Server (NTRS)

Qader, S. A. (Inventor)

1985-01-01

An improved system for recovery of a liquid hydrocarbon fuel from oil shale is presented. The oil shale pyrolysis system is composed of a retort reactor for receiving a bed of oil shale particules which are heated to pyrolyis temperature by means of a recycled solar heated gas stream. The gas stream is separated from the recovered shale oil and a portion of the gas stream is rapidly heated to pyrolysis temperature by passing it through an efficient solar heater. Steam, oxygen, air or other oxidizing gases can be injected into the recycle gas before or after the recycle gas is heated to pyrolysis temperature and thus raise the temperature before it enters the retort reactor. The use of solar thermal heat to preheat the recycle gas and optionally the steam before introducing it into the bed of shale, increases the yield of shale oil.

Method and apparatus for hydrocarbon recovery from tar sands

DOEpatents

Westhoff, James D.; Harak, Arnold E.

1989-01-01

A method and apparatus for utilizing tar sands having a broad range of bitumen content is disclosed. More particularly, tar sands are pyrolyzed in a cyclone retort with high temperature gases recycled from the cyclone retort to produce oil and hydrocarbon products. The spent tar sands are then burned at 2000.degree. F. in a burner to remove residual char and produce a solid waste that is easily disposable. The process and apparatus have the advantages of being able to utilize tar sands having a broad range of bitumen content and the advantage of producing product gases that are free from combustion gases and thereby have a higher heating value. Another important advantage is rapid pyrolysis of the tar sands in the cyclone so as to effectively utilize smaller sized reactor vessels for reducing capitol and operating costs.

In situ attosecond pulse characterization techniques to measure the electromagnetic phase

NASA Astrophysics Data System (ADS)

Spanner, M.; Bertrand, J. B.; Villeneuve, D. M.

2016-08-01

A number of techniques have been developed to characterize the attosecond emission from high-order-harmonic sources. These techniques are broadly classified as ex situ, where the attosecond pulse train photoionizes a target gas in the presence of an infrared field, and in situ, where the measurement takes place in the medium in which the attosecond pulses are generated. It is accepted that ex situ techniques measure the characteristics of the electromagnetic field, including the phase of the recombination transition moment of the emitting atom or molecule, when the phase of the second medium is known. However, there is debate about whether in situ techniques measure the electromagnetic field, or only the characteristics of the recolliding electron before recombination occurs. We show numerically that in situ measurements are not sensitive to the recombination phase, when implemented in the perturbative regime as originally envisioned, and that they do not measure the electromagnetic phase of the emission.

1. VIEW NORTH OF PARADISE MILL FOUNDATION AND TAILINGS (FEATURE ...

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

1. VIEW NORTH OF PARADISE MILL FOUNDATION AND TAILINGS (FEATURE P-7). PHOTO TAKEN FROM MERCURY RETORT. (OCTOBER, 1995) - McCormick Group Mine, Paradise Mill, East slope of Buckskin Mountain, Paradise Valley, Humboldt County, NV

30 CFR 57.22103 - Open flames (I-A, II-A, III, and V-A mines).

Code of Federal Regulations, 2010 CFR

2010-07-01

... welding, cutting, and other maintenance operations, and for igniting underground retorts in a Subcategory... after the initital test has been conducted as an alternative to the ten-minute interval testing...

2015 Subpoena and Information Request from EPA to Mercury Recyclers

EPA Pesticide Factsheets

EPA issued formal requests for information to five companies believed to be the primary recyclers/retorters and distributors of mercury in the United States to gain a better understanding of the mercury recycling marketplace.

Application of biomass pyrolytic polygeneration technology using retort reactors.

PubMed

Yang, Haiping; Liu, Biao; Chen, Yingquan; Chen, Wei; Yang, Qing; Chen, Hanping

2016-01-01

To introduce application status and illustrate the good utilisation potential of biomass pyrolytic polygeneration using retort reactors, the properties of major products and the economic viability of commercial factories were investigated. The capacity of one factory was about 3000t of biomass per year, which was converted into 1000t of charcoal, 950,000Nm(3) of biogas, 270t of woody tar, and 950t of woody vinegar. Charcoal and fuel gas had LHV of 31MJ/kg and 12MJ/m(3), respectively, indicating their potential for use as commercial fuels. The woody tar was rich in phenols, while woody vinegar contained large quantities of water and acetic acid. The economic analysis showed that the factory using this technology could be profitable, and the initial investment could be recouped over the factory lifetime. This technology offered a promising means of converting abundant agricultural biomass into high-value products. Copyright © 2015 Elsevier Ltd. All rights reserved.

High liquid yield process for retorting various organic materials including oil shale

DOEpatents

Coburn, Thomas T.

1990-01-01

This invention is a continuous retorting process for various high molecular weight organic materials, including oil shale, that yields an enhanced output of liquid product. The organic material, mineral matter, and an acidic catalyst, that appreciably adsorbs alkenes on surface sites at prescribed temperatures, are mixed and introduced into a pyrolyzer. A circulating stream of olefin enriched pyrolysis gas is continuously swept through the organic material and catalyst, whereupon, as the result of pyrolysis, the enhanced liquid product output is provided. Mixed spent organic material, mineral matter, and cool catalyst are continuously withdrawn from the pyrolyzer. Combustion of the spent organic material and mineral matter serves to reheat the catalyst. Olefin depleted pyrolysis gas, from the pyrolyzer, is enriched in olefins and recycled into the pyrolyzer. The reheated acidic catalyst is separated from the mineral matter and again mixed with fresh organic material, to maintain the continuously cyclic process.

A high liquid yield process for retorting various organic materials including oil shale

DOEpatents

Coburn, T.T.

1988-07-26

This invention is a continuous retorting process for various high molecular weight organic materials, including oil shale, that yields an enhanced output of liquid product. The organic material, mineral matter, and an acidic catalyst, that appreciably adsorbs alkenes on surface sites at prescribed temperatures, are mixed and introduced into a pyrolyzer. A circulating stream of olefin enriched pyrolysis gas is continuously swept through the organic material and catalyst, whereupon, as the result of pyrolysis, the enhanced liquid product output is provided. Mixed spent organic material, mineral matter, and cool catalyst are continuously withdrawn from the pyrolyzer. Combustion of the spent organic material and mineral matter serves to reheat the catalyst. Olefin depleted pyrolysis gas, from the pyrolyzer, is enriched in olefins and recycled into the pyrolyzer. The reheated acidic catalyst is separated from the mineral matter and again mixed with fresh organic material, to maintain the continuously cyclic process. 2 figs.

Heat penetration attributes of milkfish (Chanos chanos) thermal processed in flexible pouches: a comparative study between steam application and water immersion.

PubMed

Adepoju, Mary A; Omitoyin, Bamidele O; Mohan, Chitradurga O; Zynudheen, Aliyam A

2017-05-01

The difference in the heating penetration characteristics of product processed in retort by steam-air application and water immersion was studied. Fresh milkfish ( Chanos chanos ) packed in dry pack and in oil medium, both in flexible pouches, was thermal processed to minimum F 0 value of 7.77 at 121.1°C. Heat penetration values were recorded for each minute of processing with the aid Ellab (TM 9608, Denmark) temperature recorder. Retort come up time to achieve 121.1°C was observed to be less in steam-air which invariably led to a lower Ball's process time (B) and the total process time (T) observed in steam-air as compared to water immersion. Obtained data were plotted on a semi-logarithmic paper with temperature deficit on x -axis against time on the y -axis.

Effect of salmon type and presence/absence of bone on color, sensory characteristics, and consumer acceptability of pureed and chunked infant food products.

PubMed

DeSantos, F A; Ramamoorthi, L; Bechtel, P; Smiley, S; Brewer, M S

2010-08-01

Salmon-based infant food (puree) and toddler food (puree plus chunks) were manufactured from pink salmon, with and without bone, and from Sockeye salmon, with and without bone, to contain 45% salmon, 55% water, and 5% starch. Products were retort processed at 118 to 121 degrees C for 55 min in a steam-jacketed still retort. A trained descriptive panel (n = 7) evaluated infant and toddler foods separately. Instrumental color, pH, and water activity were also determined. Infant and toddler foods were also evaluated by a consumer panel (n = 104) of parents for product acceptability. During the manufacturing process (cooking, homogenization, retort processing), salmon infant food from pink salmon lost much of its characteristic pink color while that from sockeye salmon retained a greater amount. Bitterness was more evident in samples with bones. In the toddler food formulation containing chunks, the odor and flavor characteristics were influenced primarily by the type of salmon. The presence of bone affected visual pink color and lightness, and salmon odor only. Consumers scored products made with sockeye salmon as more acceptable despite the fact that they had more off-flavor than products from pink salmon. The appearance and thickness of the pureed infant food was more acceptable than the toddler food with chunks despite the chunky toddler product having more acceptable salmon flavor. This indicates that the color and appearance of the prototypes were the main drivers for liking. Of the total number of parents surveyed, 73% would feed this salmon product to their children.

Geotechnical centrifuge under construction

NASA Astrophysics Data System (ADS)

Richman, Barbara T.

Modifications are underway at the National Aeronautics and Space Administration (NASA) Ames Research Center in California to transform a centrifuge used in the Apollo space program to the largest geotechnical centrifuge in the free world. The centrifuge, to be finished in August and opened next January, following check out and tuning, will enable geoscientists to model stratigraphic features down to 275 m below the earth's surface. Scientists will be able to model processes that are coupled with body force loading, including earthquake response of earth structures and soil structure interaction; rubbled-bed behavior during in situ coal gasification or in oil shale in situ retorts; behavior of frozen soil; frost heave; behavior of offshore structures; wave-seabed interactions; explosive cratering; and blast-induced liquefaction.The centrifuge will have a load capacity of 900-g-tons (short); that is, it will be able to carry a net soil load of 3 short tons to a centripetal acceleration of 300 times the acceleration caused by gravity. Modified for a total cost of $2.4 million, the centrifuge will have an arm with a 7.6-m radius and a swinging platform or bucket at its end that will be able to carry a payload container measuring 2.1×2.1 m. An additional future input of $500,000 would enable the purchase of a larger bucket that could accommodate a load of up to 20 tons, according to Charles Babendreier, program director for geotechnical engineering at the National Science Foundation. Additional cooling for the motor would also be required. The centrifuge has the capability of accelerating the 20-ton load to 100 g.

77 FR 25206 - Proposed Extension of Existing Information Collection; Underground Retorts

Federal Register 2010, 2011, 2012, 2013, 2014

2012-04-27

... (those that operate within a combustible ore and either liberate methane or have the potential to liberate methane based on the history of the mine or the geological area in which the mine is located). At...

Numerical modeling of oil shale fragmentation experiments

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

Kuszmaul, J.S.

The economic development of modified in situ oil shale retorting will benefit from the ability to design a blasting scheme that creates a rubble bed of uniform permeability. Preparing such a design depends upon successfully predicting how a given explosive charge and firing sequence will fracture the oil shale. Numerical models are used to predict the extent of damage caused by a particular explosive charge. Recent single-blastwell cratering tests provided experimental measurements of the extent of damage induced by an explosion. Measuring rock damage involved crater excavation, rubble screening, crater elevation surveys, and posttest extraction of cores. These measurements weremore » compared to the damage calculated by the numerical model. Core analyses showed that the damage varied greatly from layer to layer. The numerical results also show this effect, indicating that rock damage is highly dependent on oil shale grade. The computer simulation also calculated particle velocities and dynamic stress amplitudes in the rock; predicted values agree with experimental measurements. Calculated rock fragmentation compared favorably with fragmentation measured by crater excavation and by core analysis. Because coring provides direct inspection of rock fragmentation, the use of posttest coring in future experiments is recommended.« less

77 FR 47668 - Agency Information Collection Activities; Submission for OMB Review; Comment Request; Underground...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-09

... extract oil from shale in underground metal and nonmetal I-A and I-B mines (those that operate in a... underground oil shale mines. The standard requires that, prior to ignition of underground retorts, mine...

CVD aluminiding process for producing a modified platinum aluminide bond coat for improved high temperature performance

NASA Technical Reports Server (NTRS)

Nagaraj, Bangalore A. (Inventor); Williams, Jeffrey L. (Inventor)

2003-01-01

A method of depositing by chemical vapor deposition a modified platinum aluminide diffusion coating onto a superalloy substrate comprising the steps of applying a layer of a platinum group metal to the superalloy substrate; passing an externally generated aluminum halide gas through an internal gas generator which is integral with a retort, the internal gas generator generating a modified halide gas; and co-depositing aluminum and modifier onto the superalloy substrate. In one form, the modified halide gas is hafnium chloride and the modifier is hafnium with the modified platinum aluminum bond coat comprising a single phase additive layer of platinum aluminide with at least about 0.5 percent hafnium by weight percent and about 1 to about 15 weight percent of hafnium in the boundary between a diffusion layer and the additive layer. The bond coat produced by this method is also claimed.

In Situ Activation of Microcapsules

NASA Technical Reports Server (NTRS)

Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

2000-01-01

Disclosed are microcapsules comprising a polymer shell enclosing two or more immiscible liquid phases in which a drug, or a prodrug and a drug activator are partitioned into separate phases. or prevented from diffusing out of the microcapsule by a liquid phase in which the drug is poorly soluble. Also disclosed are methods of using the microcapsules for in situ activation of drugs where upon exposure to an appropriate energy source the internal phases mix and the drug is activated in situ.

DEMONSTRATION BULLETIN: SOILTECH ANAEROBIC THERMAL PROCESSOR: OUTBOARD MARINE CORPORATION SITE

EPA Science Inventory

The ATP system is designed to desorb, collect, and recondense contaminants. The kiln contains four separate internal thermal zones: preheat, retort, combustion, and cooling. In the preheat zone, water and volatile organic compounds are vaporized. Hot solids and heavy hydrocarbons...

Characteristic and antioxidant activity of retorted gelatin hydrolysates from cobia (Rachycentron canadum) skin.

PubMed

Yang, Jing-Iong; Ho, Hsin-Yi; Chu, Yuh-Jwo; Chow, Chau-Jen

2008-09-01

Alkali-pretreated cobia (Rachycentron canadum) skin was extracted in a retort (121°C) for 30min to obtain a retorted skin gelatin hydrolysate (RSGH). The molecular mass distributions and antioxidant activities of cobia RSGH and enzyme-treated RSGHs (ET-RSGHs) derived from bromelain, papain, pancreatin, and trypsin digestion were then characterized. The molecular mass distribution of the RSGH ranged mainly between 20,000 and 700Da and those of ET-RSGHs ranged between 6500 and 700Da. The DPPH (α,α-diphenyl-β-picrylhydrazyl) radical scavenging effects (%) of 10mg/ml of RSGH and 10mg/ml of the four ET-RSGHs were 55% and 51-61%, respectively. The lipid peroxidation inhibition (%) of RSGH and ET-RSGHs (10mg/ml) were 58% and 60-71% on the fifth day in a linoleic acid model system, respectively. The 3Kd-ET-RSGHs, obtained by using a series of centrifugal ultrafiltration filters (molecular weight cut-offs of 10, 5, and 3kDa done sequentially with decreasing pore size), exhibited dramatically improved antioxidant activity, with most of the molecular mass ranging below 700Da. Compared to 10mg/ml of the RSGH, 10mg/ml of 3Kd-ET-RSGHs exhibited 45-65% more scavenging of DPPH radical and 24-38% more inhibition of lipid peroxidation. The peptides with molecular masses below 700Da in the ET-RSGHs or 3Kd-ET-RSGHs significantly affect the antioxidant properties. These peptides are composed of a small number of amino acids or free amino acids and have the potential to be added as antioxidants in foods. Copyright © 2008 Elsevier Ltd. All rights reserved.

Effect of Pre-cooking Conditions on the Quality Characteristics of Ready-To-Eat Samgyetang

PubMed Central

2015-01-01

The aim of this study was to examine the effectiveness of pre-cooking conditions on the quality characteristics of ready-to-eat (RTE) Samgyetang. Raw chickens were steamed under the different conditions of 50℃/30 min (T1), 65℃/30 min (T2), 85℃/30 min (T3), and 90℃/10 min (T4) prior to retorting at 120℃ for 65 min. The results showed that pre-cooking conditions in all treated samples could reduce fat contents in breast and leg meats by 8.5-11.7% and 10.0-11.0% compared to the control, even though there were no significant differences among treatments (p>0.05). The L* and b* values of breast and leg meats treated with the higher temperature and longer time conditions were significantly higher than the control (p<0.05), while a* values tended to decrease despite of not to a significant extent (p>0.05). Moreover, apparent viscosity and water soluble protein showed insignificant differences (p>0.05) among the samples as a result of the retorting process, which might have more negative influences on the quality. T2 samples obtained significantly the highest average Quantitative Descriptive Analysis (QDA) score and transmittance value, representing the most clear broth among the samples, compared to the control. On the other hand, T3 showed the highest cooking loss among the treatments and the lowest QDA scores among the samples. In conclusion, pre-cooking treatment prior to retorting in manufacturing Samgyetang is a plausible way to reduce its fat content. A pre-cooking condition at either 65℃ for 30 min, or 90℃ for 10 min are recommended for producing Samgyetang with optimum quality. PMID:26761871

Use of bioreactor landfill for nitrogen removal to enhance methane production through ex situ simultaneous nitrification-denitrification and in situ denitrification.

PubMed

Sun, Xiaojie; Zhang, Hongxia; Cheng, Zhaowen

2017-08-01

High concentrations of nitrate-nitrogen (NO 3 - -N) derived from ex situ nitrification phase can inhibit methane production during ex situ nitrification and in situ denitrification bioreactor landfill. A combined process comprised of ex situ simultaneous nitrification-denitrification (SND) in an aged refuse bioreactor (ARB) and in situ denitrification in a fresh refuse bioreactor (FRB) was conducted to reduce the negative effect of high concentrationsof NO 3 - -N. Ex situ SND can be achieved because NO 3 - -N concentration can be reduced and the removal rate of ammonium-nitrogen (NH 4 + -N) remains largely unchanged when the ventilation rate of ARB-A2 is controlled. The average NO 3 - -N concentrations of effluent were 470mg/L in ex situ nitrification ARB-A1 and 186mg/L in ex situ SND ARB-A2. The average NH 4 + -N removal rates of ARB-A1 and ARB-A2 were 98% and 94%, respectively. Based on the experimental data from week 4 to week 30, it is predicted that NH 4 + -N concentration in FRB-F1 of the ex situ nitrification and in situ denitrification process would reach 25mg/L after 63weeks, and about 40weeks for the FRB-F2 of ex situ SND and in situ denitrification process . Ex situ SND and in situ denitrification process can improve themethane production of FRB-F2. The lag phase time of methane production for the FRB-F2 was 11weeks. This phase was significantly shorter than the 15-week phases of FRB-F1 in ex situ nitrification and in situ denitrification process. A seven-week stabilizationphase was required to increase methane content from 5% to 50% for FRB-F2. Methane content in FRB-F1 did not reach 50% but reached the 45% peak after 20weeks. Copyright © 2017 Elsevier Ltd. All rights reserved.

[Study of the phase transformation of TiO2 with in-situ XRD in different gas].

PubMed

Ma, Li-Jing; Guo, Lie-Jin

2011-04-01

TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

43 CFR 3935.10 - Accounting records.

Code of Federal Regulations, 2012 CFR

2012-10-01

... processing plant and retort; (3) Mineral products produced and sold; (4) Shale oil products, shale gas, and... mined or processed and of all products including synthetic petroleum, shale oil, shale gas, and shale..., DEPARTMENT OF THE INTERIOR MINERALS MANAGEMENT (3000) MANAGEMENT OF OIL SHALE EXPLORATION AND LEASES...

43 CFR 3935.10 - Accounting records.

Code of Federal Regulations, 2014 CFR

2014-10-01

... processing plant and retort; (3) Mineral products produced and sold; (4) Shale oil products, shale gas, and... mined or processed and of all products including synthetic petroleum, shale oil, shale gas, and shale..., DEPARTMENT OF THE INTERIOR MINERALS MANAGEMENT (3000) MANAGEMENT OF OIL SHALE EXPLORATION AND LEASES...

43 CFR 3935.10 - Accounting records.

Code of Federal Regulations, 2013 CFR

2013-10-01

... processing plant and retort; (3) Mineral products produced and sold; (4) Shale oil products, shale gas, and... mined or processed and of all products including synthetic petroleum, shale oil, shale gas, and shale..., DEPARTMENT OF THE INTERIOR MINERALS MANAGEMENT (3000) MANAGEMENT OF OIL SHALE EXPLORATION AND LEASES...

METHOD OF CHEMICAL ANALYSIS FOR OIL SHALE WASTES

EPA Science Inventory

Several methods of chemical analysis are described for oil shale wastewaters and retort gases. These methods are designed to support the field testing of various pollution control systems. As such, emphasis has been placed on methods which are rapid and sufficiently rugged to per...

9 CFR 318.304 - Operations in the thermal processing area.

Code of Federal Regulations, 2013 CFR

2013-01-01

... factor over the specified thermal processing operation times. Temperature/time recording devices shall... minimum initial temperatures and operating procedures for thermal processing equipment, shall be posted in... available to the thermal processing system operator and the inspector. (b) Process indicators and retort...

9 CFR 318.304 - Operations in the thermal processing area.

Code of Federal Regulations, 2012 CFR

2012-01-01

... factor over the specified thermal processing operation times. Temperature/time recording devices shall... minimum initial temperatures and operating procedures for thermal processing equipment, shall be posted in... available to the thermal processing system operator and the inspector. (b) Process indicators and retort...

9 CFR 318.304 - Operations in the thermal processing area.

Code of Federal Regulations, 2014 CFR

2014-01-01

... factor over the specified thermal processing operation times. Temperature/time recording devices shall... minimum initial temperatures and operating procedures for thermal processing equipment, shall be posted in... available to the thermal processing system operator and the inspector. (b) Process indicators and retort...

9 CFR 318.304 - Operations in the thermal processing area.

Code of Federal Regulations, 2011 CFR

2011-01-01

... factor over the specified thermal processing operation times. Temperature/time recording devices shall... minimum initial temperatures and operating procedures for thermal processing equipment, shall be posted in... available to the thermal processing system operator and the inspector. (b) Process indicators and retort...

9 CFR 318.302 - Thermal processing.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 9 Animals and Animal Products 2 2011-01-01 2011-01-01 false Thermal processing. 318.302 Section 318.302 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... retort come-up operating procedures and critical factors. (2) Letters or other written communications...

A study of pyrolysis of oil shale of the Leningrad deposit by solid heat carrier

NASA Astrophysics Data System (ADS)

Gerasimov, G. Ya; Khaskhachikh, V. V.; Potapov, O. P.

2017-11-01

The investigation of the oil shale pyrolysis with a solid heat carrier was carried out using the experimental retorting system that simulates the Galoter industrial process. This system allows verifying both fractional composition of the oil shale and solid heat carrier, and their ratio and temperature. The oil shale of the Leningradsky deposit was used in the work, and quartz sand was used as the solid heat carrier. It is shown that the yield of the shale oil under the pyrolysis with solid heat carrier exceeds by more than 20% the results received in the standard Fisher retort. Using ash as the solid heat carrier results in a decrease in the yield of oil and gas with simultaneous increase in the amount of the solid residue. This is due to the chemical interaction of the acid components of the vapor-gas mixture with the oxides of alkaline-earth metals that are part of the ash.

MICROBIAL RESPONSES TO IN SITU CHEMICAL OXIDATION, SIX-PHASE HEATING, AND STEAM INJECTION REMEDIATION TECHNOLOGIES IN GROUND WATER

EPA Science Inventory

The evaluation of microbial responses to three in situ source removal remedial technologies including permanganate-based in-situ chemical oxidation (ISCO), six-phase heating (SPH), and steam injection (SI) was performed at Cape Canaveral Air Station in Florida. The investigatio...

9 CFR 318.308 - Deviations in processing.

Code of Federal Regulations, 2010 CFR

2010-01-01

...) Deviations in processing (or process deviations) must be handled according to: (1)(i) A HACCP plan for canned...) of this section. (c) [Reserved] (d) Procedures for handling process deviations where the HACCP plan... accordance with the following procedures: (a) Emergency stops. (1) When retort jams or breakdowns occur...

9 CFR 381.308 - Deviations in processing.

Code of Federal Regulations, 2010 CFR

2010-01-01

...) must be handled according to: (1)(i) A HACCP plan for canned product that addresses hazards associated... (d) of this section. (c) [Reserved] (d) Procedures for handling process deviations where the HACCP... accordance with the following procedures: (a) Emergency stops. (1) When retort jams or breakdowns occur...

118. VIEW, LOOKING SOUTHWEST OF GOLD AMALGAMATION ROOM, SHOWING AMALGAMATION ...

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

118. VIEW, LOOKING SOUTHWEST OF GOLD AMALGAMATION ROOM, SHOWING AMALGAMATION BARREL AT CENTER FOREGROUND, BULLION FURNACE IN LARGE HOOD BEHIND IT, AND GOLD RETORT IN BACKGROUND HOOD. NOTE OVERHEAD MONORAIL FOR MATERIALS HANDLING. - Shenandoah-Dives Mill, 135 County Road 2, Silverton, San Juan County, CO

43 CFR 3935.10 - Accounting records.

Code of Federal Regulations, 2011 CFR

2011-10-01

... processing plant and retort; (3) Mineral products produced and sold; (4) Shale oil products, shale gas, and... mined or processed and of all products including synthetic petroleum, shale oil, shale gas, and shale..., DEPARTMENT OF THE INTERIOR RANGE MANAGEMENT (4000) MANAGEMENT OF OIL SHALE EXPLORATION AND LEASES Production...

A "Retort Courteous."

ERIC Educational Resources Information Center

Kingsbury, Mary E.

1979-01-01

Responds to article by Pauline Wilson (School Library Journal, v25 n6 Feb 1979) in terms of defining the role of children's librarians, clarifying the goals of children's services, making a case for such services, improving the impression made by children's librarians, determining appropriate preparation, and understanding and achieving quality…

Method for in situ characterization of a medium of dispersed matter in a continuous phase

DOEpatents

Kaufman, Eric N.

1995-01-01

A method for in situ characterization of a medium of a dispersed phase in a continuous phase, including the steps of adding a fluorescent dye to one phase capable of producing fluorescence therein when the fluorescent dye is optically excited, optically exciting the fluorescent dye at a wavelength to produce fluorescence in the one phase, and monitoring the fluorescence to distinguish the continuous phase from the dispersed phase.

21 CFR 113.87 - Operations in the thermal processing room.

Code of Federal Regulations, 2012 CFR

2012-04-01

... Section 113.87 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR HUMAN CONSUMPTION THERMALLY PROCESSED LOW-ACID FOODS PACKAGED IN HERMETICALLY SEALED... Food and Drug Administration. (b) A system for product traffic control in the retort room shall be...

21 CFR 113.87 - Operations in the thermal processing room.

Code of Federal Regulations, 2011 CFR

2011-04-01

... Section 113.87 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR HUMAN CONSUMPTION THERMALLY PROCESSED LOW-ACID FOODS PACKAGED IN HERMETICALLY SEALED... Administration. (b) A system for product traffic control in the retort room shall be estab-lished to prevent...

121. FRONT ELEVATION OF TELLURIDE IRON WORKS 2.5 BY 4FOOT ...

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

121. FRONT ELEVATION OF TELLURIDE IRON WORKS 2.5 BY 4-FOOT RETORT, USED TO FLASH MERCURY FROM GOLD. MERCURY VAPOR THEN CONDENSED ON INSIDE OF HOOD AND WAS COLLECTED FOR REUSE. - Shenandoah-Dives Mill, 135 County Road 2, Silverton, San Juan County, CO

CONTROL OF SULFUR EMISSIONS FROM OIL SHALE RETORTING USING SPEND SHALE ABSORPTION

EPA Science Inventory

The paper gives results of a detailed engineering evaluation of the potential for using an absorption on spent shale process (ASSP) for controlling sulfur emissions from oil shale plants. The evaluation analyzes the potential effectiveness and cost of absorbing SO2 on combusted s...

Assessment of TAMU Rack Material in Poly Tray Racks using Spray Retort

DTIC Science & Technology

2009-07-01

FOR ADVANCED FOOD TECHNOLOGY The School of Enviromental and Biological Science Rutgers, The State University of New Jersey New Brunswick, New Jersey...A003 Mr. Henderikus B. Bruins Rutgers, The State University of New Jersey The Center for Advanced Food Technology School of Enviromental and

Letters of a Slave Turned Union Soldier.

ERIC Educational Resources Information Center

Humanities, 1990

1990-01-01

Discusses the influx of Black soldiers into the Union army following the Emancipation Proclamation. Concentrates on the case of Private Spotswood Rice. Provides a short history of Rice, including copies of Rice's letters to his enslaved daughters, the daughter's slaveholders, and an angry retort from the slaveowner to the federal commander in…

9 CFR 381.300 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... throughout the entire thermal process. (d) Canned product. A poultry food product with a water activity above...

9 CFR 381.300 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... throughout the entire thermal process. (d) Canned product. A poultry food product with a water activity above...

9 CFR 318.300 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... with a water activity above 0.85 which receives a thermal process either before or after being packed...

9 CFR 318.300 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... with a water activity above 0.85 which receives a thermal process either before or after being packed...

9 CFR 381.300 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... throughout the entire thermal process. (d) Canned product. A poultry food product with a water activity above...

9 CFR 318.300 - Definitions.

Code of Federal Regulations, 2011 CFR

2011-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... with a water activity above 0.85 which receives a thermal process either before or after being packed...

9 CFR 318.300 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... with a water activity above 0.85 which receives a thermal process either before or after being packed...

9 CFR 381.300 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... throughout the entire thermal process. (d) Canned product. A poultry food product with a water activity above...

9 CFR 381.300 - Definitions.

Code of Federal Regulations, 2011 CFR

2011-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... throughout the entire thermal process. (d) Canned product. A poultry food product with a water activity above...

9 CFR 318.300 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-01-01

... of air from a retort before the start of process timing. (x) Water activity. The ratio of the water vapor pressure of the product to the vapor pressure of pure water at the same temperature. ... with a water activity above 0.85 which receives a thermal process either before or after being packed...

7 CFR 98.2 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-01-01

..., READY-TO-EAT (MRE's), MEATS, AND MEAT PRODUCTS MRE's, Meats, and Related Meat Food Products § 98.2... acceptable one meal serving, retorted pouched or 18-24 serving hermetically-sealed tray packed meat, or meal... operational food rations, and as an item of general issue by the military. Meat. This includes the edible part...

Optimizing single-nanoparticle two-photon microscopy by in situ adaptive control of femtosecond pulses

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

Li, Donghai; Deng, Yongkai; Chu, Saisai

2016-07-11

Single-nanoparticle two-photon microscopy shows great application potential in super-resolution cell imaging. Here, we report in situ adaptive optimization of single-nanoparticle two-photon luminescence signals by phase and polarization modulations of broadband laser pulses. For polarization-independent quantum dots, phase-only optimization was carried out to compensate the phase dispersion at the focus of the objective. Enhancement of the two-photon excitation fluorescence intensity under dispersion-compensated femtosecond pulses was achieved. For polarization-dependent single gold nanorod, in situ polarization optimization resulted in further enhancement of two-photon photoluminescence intensity than phase-only optimization. The application of in situ adaptive control of femtosecond pulse provides a way for object-orientedmore » optimization of single-nanoparticle two-photon microscopy for its future applications.« less

Combined In-Situ XRD and In-Situ XANES Studies on the Reduction Behavior of a Rhenium Promoted Cobalt Catalyst

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

Kumar, Nitin; Payzant, E Andrew; Jothimurugesan, K

2011-01-01

A 10% Co 4% Re/(2% Zr/SiO2) catalyst was prepared by co-impregnation using a silica support modified by 2% Zr. The catalyst was characterized by temperature programmed reduction (TPR), in situ XRD and in situ XANES analysis where it was simultaneously exposed to H2 using a temperature programmed ramp. The results showed the two step reduction of large crystalline Co3O4 with CoO as an intermediate. TPR results showed that the reduction of highly dispersed Co3O4 was facilitated by reduced rhenium by a H2-spillover mechanism. In situ XRD results showed the presence of both, Co-hcp and Co-fcc phases in the reduced catalystmore » at 400 C. However, the Co-hcp phase was more abundant, which is thought to be the more active phase as compared to the Co-fcc phase for CO hydrogenation. CO hydrogenation at 270 C and 5 bar pressure produces no detectable change in the phases during the time of experiment. In situ XANES results showed a decrease in the metallic cobalt in the presence of H2/CO, which can be attributed due to oxidation of the catalyst by reaction under these conditions.« less

Water resources and potential hydrologic effects of oil-shale development in the southeastern Uinta Basin, Utah and Colorado

USGS Publications Warehouse

Lindskov, K.L.; Kimball, B.A.

1984-01-01

Proposed oil-shale mining in northeastern Utah is expected to impact the water resources of a 3,000-square-mile area. This report summarizes a comprehensive hydrologic investigation of the area which resulted in 13 published reports. Hydrologic information obtained during 1974-80 was used to evaluate the availability of water and to evaluate potential impacts of an oil-shale industry on the water resources.The study area is the southeastern part of the Uinta Basin, Utah and Colorado, where the hydrology is extremely variable. The normal annual precipitation averages 11 inches and varies with altitude. It ranges from less than 8 inches at altitudes below 5,000 feet along the White and Green Rivers to more than 20 inches where altitudes exceed 9,000 feet on the Roan Plateau.The White and Green Rivers are large streams that flow through the area. They convey an average flow of 4.3 million acre-feet per year from outside drainage areas of about 34,000 square miles, which is more than 150 times as much flow as that originating within the area. Streams originating in areas where precipitation is less than 10 inches are ephemeral. Mean annual runoff from the study area is about 28,000 acre-feet and ranges from less than 0.1 to 1.6 inches, depending on the location. At any given site, runoff varies greatly-from year to year and season to season. Potential evapotranspiration is large, exceeding precipitation in all years. Three major aquifers occur in the area. They are alluvial deposits of small areal extent along the major stream valleys; the bird's-nest aquifer of the Parachute Creek Member of the Green River Formation, which is limited to the central part of the study area; and the Douglas Creek aquifer of the Douglas Creek Member of the Green River Formation, which underlies most of the area. Total recoverable water in storage in the three aquifers is about 18 million acre-feet. Yields of individual wells and interference between wells limit the maximum practical withdrawal to about 20,000 acre-feet per year.An oil-shale industry in the southeastern Uinta Basin with a peak production of 400,000 barrels of oil per day would require a water supply of about 70,000 acre-feet per year. Sources of water supply considered for such an industry were: diversion from the natural flow of the White River, a proposed reservoir on the White River, diversion from the White River combined with proposed off-stream storage in Hells Hole Canyon, diversion from the Green River, and conjunctive use of ground and surface water.The proposed reservoir on the White River would trap about 90 percent of the sediment moving in the river and in turn would release almost sediment-free water. Possible impacts are changes in channel gradient in the downstream 18 miles of the White River and changes in bank stability. In some parts of the area, annual sheet-erosion rates are as great as 2.2 acre-feet per square mile but sediment yield to the White River is less than might be expected because the runoff is small. If process water from retort operations or water used in the construction of surface facilities is discharged into a normally dry streambed, increased channel erosion and sediment in tributary streams could result in increased sediment loads in the White River. In addition, sediment yields from retorted-shale piles with minimum slopes could exceed 0.1 acrefoot per square mile during a common storm. Thus, without safeguards, the useful life of any proposed reservoir or holding pond could be decreased considerably.Leachate water from retorted-shale piles has large concentrations of sodium and sulfate, and the chemical composition of retort waters differs considerably from that of the natural waters of the area. The retort waters contain a greater concentration of dissolved solids and more organic carbon and nutrients. Without proper disposal or impoundment of retort and leachate waters, the salinity of downstream waters in the Colorado River Basin would be increased.

In situ monitoring of liquid phase electroepitaxial growth

NASA Technical Reports Server (NTRS)

Okamoto, A.; Isozumi, S.; Lagowski, J.; Gatos, H. C.

1982-01-01

In situ monitoring of the layer thickness during liquid phase electroepitaxy (LPEE) was achieved with a submicron resolution through precise resistance measurements. The new approach to the study and control of LPEE was applied to growth of undoped and Ge-doped GaAs layers. The in situ determined growth kinetics was found to be in excellent agreement with theory.

A novel energy-efficient pyrolysis process: self-pyrolysis of oil shale triggered by topochemical heat in a horizontal fixed bed.

PubMed

Sun, You-Hong; Bai, Feng-Tian; Lü, Xiao-Shu; Li, Qiang; Liu, Yu-Min; Guo, Ming-Yi; Guo, Wei; Liu, Bao-Chang

2015-02-06

This paper proposes a novel energy-efficient oil shale pyrolysis process triggered by a topochemical reaction that can be applied in horizontal oil shale formations. The process starts by feeding preheated air to oil shale to initiate a topochemical reaction and the onset of self-pyrolysis. As the temperature in the virgin oil shale increases (to 250-300°C), the hot air can be replaced by ambient-temperature air, allowing heat to be released by internal topochemical reactions to complete the pyrolysis. The propagation of fronts formed in this process, the temperature evolution, and the reaction mechanism of oil shale pyrolysis in porous media are discussed and compared with those in a traditional oxygen-free process. The results show that the self-pyrolysis of oil shale can be achieved with the proposed method without any need for external heat. The results also verify that fractured oil shale may be more suitable for underground retorting. Moreover, the gas and liquid products from this method were characterised, and a highly instrumented experimental device designed specifically for this process is described. This study can serve as a reference for new ideas on oil shale in situ pyrolysis processes.

A Novel Energy-Efficient Pyrolysis Process: Self-pyrolysis of Oil Shale Triggered by Topochemical Heat in a Horizontal Fixed Bed

PubMed Central

Sun, You-Hong; Bai, Feng-Tian; Lü, Xiao-Shu; Li, Qiang; Liu, Yu-Min; Guo, Ming-Yi; Guo, Wei; Liu, Bao-Chang

2015-01-01

This paper proposes a novel energy-efficient oil shale pyrolysis process triggered by a topochemical reaction that can be applied in horizontal oil shale formations. The process starts by feeding preheated air to oil shale to initiate a topochemical reaction and the onset of self-pyrolysis. As the temperature in the virgin oil shale increases (to 250–300°C), the hot air can be replaced by ambient-temperature air, allowing heat to be released by internal topochemical reactions to complete the pyrolysis. The propagation of fronts formed in this process, the temperature evolution, and the reaction mechanism of oil shale pyrolysis in porous media are discussed and compared with those in a traditional oxygen-free process. The results show that the self-pyrolysis of oil shale can be achieved with the proposed method without any need for external heat. The results also verify that fractured oil shale may be more suitable for underground retorting. Moreover, the gas and liquid products from this method were characterised, and a highly instrumented experimental device designed specifically for this process is described. This study can serve as a reference for new ideas on oil shale in situ pyrolysis processes. PMID:25656294

Method for in situ characterization of a medium of dispersed matter in a continuous phase

DOEpatents

Kaufman, E.N.

1995-03-07

A method is described for the in situ characterization of a medium of a dispersed phase in a continuous phase, including the steps of adding a fluorescent dye to one phase capable of producing fluorescence therein when the fluorescent dye is optically excited, optically exciting the fluorescent dye at a wavelength to produce fluorescence in the one phase, and monitoring the fluorescence to distinguish the continuous phase from the dispersed phase. 2 figs.

21 CFR 113.40 - Equipment and procedures.

Code of Federal Regulations, 2011 CFR

2011-04-01

... ensure a supply of clean, dry air. (3) Pressure gages. Each retort should be equipped with a pressure... should have adequate filter systems to ensure a supply of clean, dry air. (3) Pressure gages. (i) Each... controllers should have adequate filter systems to ensure a supply of clean, dry air. (3) Pressure gages. Each...

Retort to Religious Critics of RET.

ERIC Educational Resources Information Center

Nardi, Thomas J.

This paper is concerned with people who contact clergymen for counseling who could benefit from the short-term directive therapeutic approach of Rational Emotive Therapy (RET) and the reluctance of clergymen to use RET. The integration of the precepts of Christianity and the concepts of RET is considered. This paper is specifically a response to…

9 CFR 318.305 - Equipment and procedures for heat processing systems.

Code of Federal Regulations, 2011 CFR

2011-01-01

... ensure a supply of clean, dry air. The recorder timing mechanism shall be accurate. (i) Chart-type... filter systems to ensure a supply of clean, dry air. (ii) Pressure recording device. Each retort shall be... section. (2) Cooling canal water shall be chlorinated or treated with a chemical approved by the...

9 CFR 381.305 - Equipment and procedures for heat processing systems.

Code of Federal Regulations, 2011 CFR

2011-01-01

... supply of clean, dry air. The recorder timing mechanism shall be accurate. (i) Chart-type devices... filter systems to ensure a supply of clean, dry air. (ii) Pressure recording device. Each retort shall be... cooling except as provided for in paragraphs (h) (2) and (3) of this section. (2) Cooling canal water...

In situ investigations of the phase change behaviour of tungsten oxide nanostructures.

PubMed

Thummavichai, Kunyapat; Wang, Nannan; Xu, Fang; Rance, Graham; Xia, Yongda; Zhu, Yanqiu

2018-04-01

This study uses two in situ techniques to investigate the geometry and phase change behaviour of bundled ultrathin W 18 O 49 nanowires and WO 3 nanoparticles. The in situ X-ray diffraction (XRD) results have shown that the phase transition of WO 3 nanoparticles occurs in sequence from monoclinic (room temperature) → orthorhombic (350°C) → tetragonal (800°C), akin to bulk WO 3 ; however, W 18 O 49 nanowires remain stable as the monoclinic phase up to 500°C, after which a complete oxidation to WO 3 and transformation to the orthorhombic β-phase at 550°C is observed. The in situ Raman spectroscopy investigations have revealed the Raman peak downshifts as the temperature increases, and have identified the 187.6 cm -1 as the fingerprint band for the phase transition from γ- to β-phase of the WO 3 nanoparticle. Furthermore, WO 3 nanoparticles exhibit the γ- to β-phase conversion at 275°C, which is about 75°C lower than the relaxation temperature of 350°C for the monoclinic γ-W 18 O 49 nanowires. These new fundamental understandings on the phase transition behaviour offer important guidance for the design and development of tungsten oxide-based nanodevices by defining their allowed operating conditions.

In situ investigations of the phase change behaviour of tungsten oxide nanostructures

NASA Astrophysics Data System (ADS)

Thummavichai, Kunyapat; Wang, Nannan; Xu, Fang; Rance, Graham; Xia, Yongda; Zhu, Yanqiu

2018-04-01

This study uses two in situ techniques to investigate the geometry and phase change behaviour of bundled ultrathin W18O49 nanowires and WO3 nanoparticles. The in situ X-ray diffraction (XRD) results have shown that the phase transition of WO3 nanoparticles occurs in sequence from monoclinic (room temperature) → orthorhombic (350°C) → tetragonal (800°C), akin to bulk WO3; however, W18O49 nanowires remain stable as the monoclinic phase up to 500°C, after which a complete oxidation to WO3 and transformation to the orthorhombic β-phase at 550°C is observed. The in situ Raman spectroscopy investigations have revealed the Raman peak downshifts as the temperature increases, and have identified the 187.6 cm-1 as the fingerprint band for the phase transition from γ- to β-phase of the WO3 nanoparticle. Furthermore, WO3 nanoparticles exhibit the γ- to β-phase conversion at 275°C, which is about 75°C lower than the relaxation temperature of 350°C for the monoclinic γ-W18O49 nanowires. These new fundamental understandings on the phase transition behaviour offer important guidance for the design and development of tungsten oxide-based nanodevices by defining their allowed operating conditions.

In situ phase transformation of Laves phase from Chi-phase in Mo-containing Fe–Cr–Ni alloys

DOE PAGES

Tan, L.; Yang, Y.

2015-11-01

For an in situ phase transformation of the Chi (χ) phase to the Laves phase we observed in a Fe–Cr–Ni–Mo model alloy. The morphology, composition, and crystal structure of the χ and Laves phases, and their orientation relationship with the matrix austenite phase were investigated. The resulted Laves phase has larger lattice mismatch with the matrix phase than the χ phase, leading to the increase of local strain fields and the formation of dislocations. Moreover, this finding is helpful to understand the precipitation behavior of the intermetallic phases in the Mo-containing austenitic stainless steels.

Calculation of Ceramic Phase Diagrams

DTIC Science & Technology

1979-11-30

Recent examples of the use of data bases and computer techniques in solw~ng problems associated with: in-situ formation of columbium, nickel and...examples of the use of data bases and computer techniques in solving problems associated with: in-situ formation of columbium, nickel and cobalt based...covers processing of in-situ eutectic composite formation in columbium, nickel and cobalt base superalloys, sigma phase formation in high temperature

In situ diffusion experiment in granite: Phase I

NASA Astrophysics Data System (ADS)

Vilks, P.; Cramer, J. J.; Jensen, M.; Miller, N. H.; Miller, H. G.; Stanchell, F. W.

2003-03-01

A program of in situ experiments, supported by laboratory studies, was initiated to study diffusion in sparsely fractured rock (SFR), with a goal of developing an understanding of diffusion processes within intact crystalline rock. Phase I of the in situ diffusion experiment was started in 1996, with the purpose of developing a methodology for estimating diffusion parameter values. Four in situ diffusion experiments, using a conservative iodide tracer, were performed in highly stressed SFR at a depth of 450 m in the Underground Research Laboratory (URL). The experiments, performed over a 2 year period, yielded rock permeability estimates of 2×10 -21 m 2 and effective diffusion coefficients varying from 2.1×10 -14 to 1.9×10 -13 m 2/s, which were estimated using the MOTIF code. The in situ diffusion profiles reveal a characteristic "dog leg" pattern, with iodide concentrations decreasing rapidly within a centimeter of the open borehole wall. It is hypothesized that this is an artifact of local stress redistribution and creation of a zone of increased constrictivity close to the borehole wall. A comparison of estimated in situ and laboratory diffusivities and permeabilities provides evidence that the physical properties of rock samples removed from high-stress regimes change. As a result of the lessons learnt during Phase I, a Phase II in situ program has been initiated to improve our general understanding of diffusion in SFR.

Crystallization of spray-dried lactose/protein mixtures in humid air

NASA Astrophysics Data System (ADS)

Shawqi Barham, A.; Kamrul Haque, Md.; Roos, Yrjö H.; Kieran Hodnett, B.

2006-10-01

An in situ crystallization technique with X-ray diffraction analysis complemented by ex situ scanning electron microscopy and chromatographic analysis of the α/( α+ β) solid-state anomeric ratios has been developed to study the crystallization of lactose/protein mixtures in humid air. This technique was used to determine changes in phase composition and morphology during crystallization. Following an induction period during which water is sorbed, crystallization is rapid and the predominant phase observed using the in situ method in spray-dried lactose/sodium-caseinate, albumin and gelatin is α-lactose monohydrate. However, in the case of spray-dried lactose/whey protein isolate (WPI) the predominant phase that appears is the α/ β mixed phase with smaller amounts of α-lactose monohydrate. With pure lactose the α/ β mixed phase appears as a transient shortly after the onset of crystallization and α-lactose monohydrate and β-lactose both appear as stable crystalline phases at longer times. Another transient phase with 2 θ=12.2°, 20.7° and 21.8° was observed in spray-dried lactose/albumin. This phase decomposed as α-lactose monohydrate developed. Three phases seem to persist in the case of spray-dried lactose/gelatin, namely the phase with peaks at 2 θ=12.2°, 20.7° and 21.8°, α-lactose monohydrate and β-lactose for the duration of the in situ experiment.

Phase separation of in situ forming poly (lactide-co-glycolide acid) implants investigated using a hydrogel-based subcutaneous tissue surrogate and UV-vis imaging.

PubMed

Sun, Yu; Jensen, Henrik; Petersen, Nickolaj J; Larsen, Susan W; Østergaard, Jesper

2017-10-25

Phase separation of in situ forming poly (lactide-co-glycolide acid) (PLGA) implants with agarose hydrogels as the provider of nonsolvent (water) mimicking subcutaneous tissue was investigated using a novel UV-vis imaging-based analytical platform. In situ forming implants of PLGA-1-methyl-2-pyrrolidinone and PLGA-triacetin representing fast and slow phase separating systems, respectively, were evaluated using this platform. Upon contact with the agarose hydrogel, the phase separation of the systems was followed by the study of changes in light transmission and absorbance as a function of time and position. For the PLGA-1-methyl-2-pyrrolidinone system, the rate of spatial phase separation was determined and found to decrease with increasing the PLGA concentration from 20% to 40% (w/w). Hydrogels with different agarose concentrations (1% and 10% (w/v)) were prepared for providing the nonsolvent, water, to the in situ forming PLGA implants simulating the injection site environment. The resulting implant morphology depended on the stiffness of hydrogel matrix, indicating that the matrix in which implants are formed is of importance. Overall, the work showed that the UV-vis imaging-based platform with an agarose hydrogel mimicking the subcutaneous tissue holds potential in providing bio-relevant and mechanistic information on the phase separation processes of in situ forming implants. Copyright © 2017 Elsevier B.V. All rights reserved.

When the "Asked for" Becomes the "Not Wanted:" A Grant Funder's Retort to a Foster Care Multiple Case Study

ERIC Educational Resources Information Center

Palladino, John M.; Giesler, Mark A.

2012-01-01

A significant population of foster care infants and toddlers access early special education services under the parameters of the Individuals with Disabilities Education Act (IDEA)-Part C. A dearth of literature exists about special education interventionists' services for this particular population. In response, we conducted a government-funded…

Retort Upgrading for Surge

DTIC Science & Technology

2008-11-01

Endress & Hauser Analog Level Gauge PV with Sight Glass Minco Temperature Transmitters (2) Steam Pressure Alarm Switch ABB Kent Taylor...Transmitter SV (0-100 psig range) LogTec Pressure Transmitter PV (0-60 psig) Strobe Light Rotor Proximity Switches (3) Endress & Hauser ... Endress & Hauser Analog Level Gauge PV with Sight Glass Minco Temperature Transmitters (2) Steam Pressure Alarm Switch ABB Kent Taylor

Identification and Development of Simple Acceptance Tests for MRE Film Pouch Materials

DTIC Science & Technology

2006-01-26

retort applications, such as wheat snack bread, shortbread cookies, and beef jerky. Film #2 (48 GA PET/10#PE/.00035F/2 mil sealant) was chosen as the...for polymers) is the melt flow direction and its relation to the direction of the scratch test. It is known that, when polymers are molded or extruded

"As a Shepherd Divideth His Sheep from the Goats": Does the Daily Spiritual Experiences Scale Encapsulate Separable Theistic and Civility Components?

ERIC Educational Resources Information Center

Schuurmans-Stekhoven, James Benjamin

2013-01-01

Numerous studies suggest spirituality and subjective well-being (SWB) are positively associated. However, critics argue that popular spirituality instruments--including the Daily Spiritual Experiences Scale (DSES)--contain items that conflate religiosity/spirituality (R/S), prosociality and SWB. Advocates of the DSES retort that, despite this…

Sea-based Fuel Synthesis Work at NRL from FY02 to FY07 (October 2001 - October 2006)

DTIC Science & Technology

2010-08-05

nearly a decade and involved every aspect of the development of a new liquid hydrocarbon from shale including mining, retorting , refining, performance...the end of each year’s effort. This was an attempt by Willauer and Hardy to obtain the necessary total funding package to accelerate the carbon

9 CFR 381.305 - Equipment and procedures for heat processing systems.

Code of Federal Regulations, 2014 CFR

2014-01-01

... plates. Whenever one or more divider plates are used between any two layers of containers or placed on... from several still retorts shall lead to the atmosphere. The manifold header shall not be controlled by...) Venting through multiple 1 inch (2.5 cm) vents discharging directly to the atmosphere. EC11SE91.047...

9 CFR 381.305 - Equipment and procedures for heat processing systems.

Code of Federal Regulations, 2012 CFR

2012-01-01

... plates. Whenever one or more divider plates are used between any two layers of containers or placed on... from several still retorts shall lead to the atmosphere. The manifold header shall not be controlled by...) Venting through multiple 1 inch (2.5 cm) vents discharging directly to the atmosphere. EC11SE91.047...

9 CFR 381.305 - Equipment and procedures for heat processing systems.

Code of Federal Regulations, 2013 CFR

2013-01-01

... plates. Whenever one or more divider plates are used between any two layers of containers or placed on... from several still retorts shall lead to the atmosphere. The manifold header shall not be controlled by...) Venting through multiple 1 inch (2.5 cm) vents discharging directly to the atmosphere. EC11SE91.047...

Simplifying pyrolysis; using gasification to produce corn stover and wheat straw biochar for sorptive and horitcultural media

USDA-ARS?s Scientific Manuscript database

Biochar is a renewable, useful material that can be utilized in many different applications. Biochar is commonly produced via pyrolysis methods using a retort-style oven with inert gas. Gasification is another method that can utilize pyrolysis to produce biochar, but with the advantage of not requir...

TREATMENT OF FISSION PRODUCT WASTE

DOEpatents

Huff, J.B.

1959-07-28

A pyrogenic method of separating nuclear reactor waste solutions containing aluminum and fission products as buring petroleum coke in an underground retort, collecting the easily volatile gases resulting as the first fraction, he uminum chloride as the second fraction, permitting the coke bed to cool and ll contain all the longest lived radioactive fission products in greatly reduced volume.

Vertical phase separation in bulk heterojunction solar cells formed by in situ polymerization of fulleride

PubMed Central

Zhang, Lipei; Xing, Xing; Zheng, Lingling; Chen, Zhijian; Xiao, Lixin; Qu, Bo; Gong, Qihuang

2014-01-01

Vertical phase separation of the donor and the acceptor in organic bulk heterojunction solar cells is crucial to improve the exciton dissociation and charge transport efficiencies. This is because whilst the exciton diffusion length is limited, the organic film must be thick enough to absorb sufficient light. However, it is still a challenge to control the phase separation of a binary blend in a bulk heterojunction device architecture. Here we report the realization of vertical phase separation induced by in situ photo-polymerization of the acrylate-based fulleride. The power conversion efficiency of the devices with vertical phase separation increased by 20%. By optimising the device architecture, the power conversion efficiency of the single junction device reached 8.47%. We believe that in situ photo-polymerization of acrylate-based fulleride is a universal and controllable way to realise vertical phase separation in organic blends. PMID:24861168

FIELD IMPLEMENTATION OF A WINSOR TYPE I SURFACTANT/ALCOHOL MIXTURE FOR IN SITU SOLUBILIZATION OF A COMPLEX LNAPL AS A SINGLE-PHASE MICROEMULSION

EPA Science Inventory

A Winsor Type I surfactant/alcohol mixture was used as an in situ flushing agent to solubilize a muticomponent nonaqueous phase liquid (NAPL) as a single-phase microemulsion (SPME) in a hydraulically isolated test cell at Hill Air Force Base (AFB), Utah. The surfactant (polyoxye...

Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions

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

Chandran, Ravi

In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energymore » storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO 2 and in graphite/LiMn 2O 4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced by mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean α-phase. These experiments have been performed at CG-1D Neutron Imaging Prototype Station at SNS.« less

In situ TEM observation of FCC Ti formation at elevated temperatures

DOE PAGES

Yu, Qian; Kacher, Josh; Gammer, Christoph; ...

2017-07-04

Pure Ti traditionally exhibits the hexagonal closed packed (HCP) crystallographic structure under ambient conditions and the body centered cubic (BCC) structure at elevated temperatures. In addition to these typical structures for Ti alloys, the presence of a face centered cubic (FCC) phase associated with thin films, interfaces, or high levels of plastic deformation has occasionally been reported. Here in this paper we show that small FCC precipitates form in freestanding thin foils during in situ transmission electron microscope (TEM) heating and we discuss the potential origins of the FCC phase in light of the in situ observations. This FCC phasemore » was found to be stable upon cooling and under ambient conditions, which allowed us to explore its mechanical properties and stability via nanomechanical in situ TEM testing. It was found that FCC platelets within the HCP matrix phase were stable under mechanical deformation and exhibited similar mechanical deformation behavior as the parent HCP phase.« less

Roles of strain and domain boundaries on the phase transition stability of VO2 thin films

NASA Astrophysics Data System (ADS)

Jian, Jie; Chen, Aiping; Chen, Youxing; Zhang, Xinghang; Wang, Haiyan

2017-10-01

The fundamental phase transition mechanism and the stability of the semiconductor-to-metal phase transition properties during multiple thermal cycles have been investigated on epitaxial vanadium dioxide (VO2) thin films via both ex situ heating and in situ heating by transmission electron microscopy (TEM). VO2 thin films were deposited on c-cut sapphire substrates by pulsed laser deposition. Ex situ studies show the broadening of transition sharpness (ΔT) and the width of thermal hysteresis (ΔH) after 60 cycles. In situ TEM heating studies reveal that during thermal cycles, large strain was accumulated around the domain boundaries, which was correlated with the phase transition induced lattice constant change and the thermal expansion. It suggests that the degradation of domain boundary structures in the VO2 films not only caused the transition property reduction (e.g., the decrease in ΔT and ΔH) but also played an important role in preventing the film from fracture during thermal cycles.

In situ TEM observation of FCC Ti formation at elevated temperatures

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

Yu, Qian; Kacher, Josh; Gammer, Christoph

Pure Ti traditionally exhibits the hexagonal closed packed (HCP) crystallographic structure under ambient conditions and the body centered cubic (BCC) structure at elevated temperatures. In addition to these typical structures for Ti alloys, the presence of a face centered cubic (FCC) phase associated with thin films, interfaces, or high levels of plastic deformation has occasionally been reported. Here in this paper we show that small FCC precipitates form in freestanding thin foils during in situ transmission electron microscope (TEM) heating and we discuss the potential origins of the FCC phase in light of the in situ observations. This FCC phasemore » was found to be stable upon cooling and under ambient conditions, which allowed us to explore its mechanical properties and stability via nanomechanical in situ TEM testing. It was found that FCC platelets within the HCP matrix phase were stable under mechanical deformation and exhibited similar mechanical deformation behavior as the parent HCP phase.« less

The metal-insulator transition in a phase-separated manganite studied by in situ STS

NASA Astrophysics Data System (ADS)

Snijders, P. C.; Gao, M.; Guo, H.; Ward, T. Z.; Gao, H.-J.; Shen, J.; Gai, Z.

2012-02-01

Electronic phase separation (EPS) is a key feature at the heart of the wide variety of electronic and magnetic properties in complex oxides. One consequence of EPS is that electronic transport experiments in bulk materials or 2D films mostly probe the low resistivity electronic phases due to the percolative path of the current. We study oxygen deficient La5/8-xPrxCa3/8M nO3 (LPCMO) thin films using both in situ scanning tunneling spectroscopy (STS) and ex situ transport experiments. The oxygen deficiency is known to decrease the metal-insulator transition (MIT) temperature or even completely suppress the MIT in conventional transport experiments. We show that in situ STS is able to detect the MIT even in systems where conventional transport experiments do not show an MIT at zero magnetic field.

In Situ Chemical Characterization of Mineral Phases in Lunar Granulite Meteorite Northwest Africa 5744

NASA Astrophysics Data System (ADS)

Kent, J. J.; Brandon, A. D.; Lapen, T. J.; Peslier, A. H.; Irving, A. J.; Coleff, D. M.

2012-03-01

NWA 5744 is compared to other magnesian lunar granulites by the chemistry of situ phases and aided by a CT density volume. NWA 5744 may be linked to FAN composition materials, and magnesian granulites as a whole probably have diverse origins.

Bibliography of Technical Publications and Papers. October 1987-September 1988

DTIC Science & Technology

1990-07-01

LATE, K. G. Production of retorted meals in coextrud,-A barrier trays. Wornick Services, Inc., Contract No. DAAK60-87-C-0050. NATICK/IT-88/060...Schultz, G. 105 Meiselman, H./ H. L. 3, 96, 97 Seasholtz, S. 45 98, 122, 123 Seefeldt , V. D. 126 Mello, J. 43 Sharp, R./ R. K. 66, 92 Monaghan, P. B. 33

Gas stream cleaning system and method

DOEpatents

Kunchal, S. Kumar; Erck, Louis J.; Harris, Harry A.

1979-04-13

An oil mist and solid particle laden gas from an oil shale retorting operation is initially treated with a temperature controlled oil spray and then by a coalescer to reduce the quantity of oil mist and remove most of the solid particle content of the gas stream and then finally treated by an electrostatic precipitator to essentially remove the oil mist remaining in the gas.

78 FR 39313 - Notice of Intent To Prepare an Environmental Impact Statement for the Enefit American Oil Utility...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-07-01

..., 8 miles of natural gas supply pipeline, 10 miles of oil product line, 29 miles of single or dual... commercial oil shale mining, retorting, and upgrading operation located in Uintah County, Utah. Approval or... 13X] Notice of Intent To Prepare an Environmental Impact Statement for the Enefit American Oil Utility...

Improving packaged food quality and safety. Part 1: synchrotron X-ray analysis.

PubMed

López-Rubio, A; Hernandez-Muñoz, P; Catala, R; Gavara, R; Lagarón, J M

2005-10-01

The objective was to demonstrate, as an example of an application, the potential of synchrotron X-ray analysis to detect morphological alterations that can occur in barrier packaging materials and structures. These changes can affect the packaging barrier characteristics when conventional food preservation treatments are applied to packaged food. The paper presents the results of a number of experiments where time-resolved combined wide-angle X-ray scattering and small-angle X-ray scattering analysis as a function of temperature and humidity were applied to ethylene-vinyl alcohol co-polymers (EVOH), polypropylene (PP)/EVOH/PP structures, aliphatic polyketone terpolymer (PK) and amorphous polyamide (aPA) materials. A comparison between conventional retorting and high-pressure processing treatments in terms of morphologic alterations are also presented for EVOH. The impact of retorting on the EVOH structure contrasts with the good behaviour of the PK during this treatment and with that of aPA. However, no significant structural changes were observed by wide-angle X-ray scattering in the EVOH structures after high-pressure processing treatment. These structural observations have also been correlated with oxygen permeability measurements that are of importance when guaranteeing the intended levels of safety and quality of packaged food.

Self-cementing properties of oil shale solid heat carrier retorting residue.

PubMed

Talviste, Peeter; Sedman, Annette; Mõtlep, Riho; Kirsimäe, Kalle

2013-06-01

Oil shale-type organic-rich sedimentary rocks can be pyrolysed to produce shale oil. The pyrolysis of oil shale using solid heat carrier (SHC) technology is accompanied by large amount of environmentally hazardous solid residue-black ash-which needs to be properly landfilled. Usage of oil shale is growing worldwide, and the employment of large SHC retorts increases the amount of black ash type of waste, but little is known about its physical and chemical properties. The objectives of this research were to study the composition and self-cementing properties of black ash by simulating different disposal strategies in order to find the most appropriate landfilling method. Three disposal methods were simulated in laboratory experiment: hydraulic disposal with and without grain size separation, and dry dumping of moist residue. Black ash exhibited good self-cementing properties with maximum compressive strength values of >6 MPa after 90 days. About 80% of strength was gained in 30 days. However, the coarse fraction (>125 µm) did not exhibit any cementation, thus the hydraulic disposal with grain size separation should be avoided. The study showed that self-cementing properties of black ash are governed by the hydration of secondary calcium silicates (e.g. belite), calcite and hydrocalumite.

Effects of stripped oil shale retort water on fishes, birds, and mammals

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

Nystrom, R.R.

1983-01-01

Golden hamsters (Mesocricetus auratus Water), coturnix quail (Coturnix coturnix Teminck and Schlegal), fathead minnows (Pimphales promelas Rafinesque), and rainbow trout (Salmo gairdneri Richardson) were subjected to various exposures of stripped oil shale retort water (SRW). Chronic low-level exposures of all experimental animals to SRW revealed no adverse histological effects attributable to SRW. Also, production and development of second generation fathead minnows and coturnix quail exposed to SRW was normal. Subacute exposure of rainbow trout to SRW produced ultrastructural changes detected by transmission, scanning, and freeze fracture electron microscopy) in the gill, liver, and kidney tissues. The gills showed a swellingmore » of secondary lamellae, disorganization of normal tissue architecture, and sloughing of respiratory cells. The liver contained lamellar bodies not seen in the controls. Relatively large, electron dense, membrane-bounded deposits were present in proximal tubule cells of the kidney. Sodium arsenite (a significant component of SRW) was shown to cause swelling of granular endosplasmic reticulum in quail liver tissue with an acute exposure. This effect could be related to the fact that arsenic inhibits ATP production, which would decrease the ability of the sodium pumps to maintain a normal osmotic balance.« less

Molecular characterization and comparison of shale oils generated by different pyrolysis methods

USGS Publications Warehouse

Birdwell, Justin E.; Jin, Jang Mi; Kim, Sunghwan

2012-01-01

Shale oils generated using different laboratory pyrolysis methods have been studied using standard oil characterization methods as well as Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) with electrospray ionization (ESI) and atmospheric photoionization (APPI) to assess differences in molecular composition. The pyrolysis oils were generated from samples of the Mahogany zone oil shale of the Eocene Green River Formation collected from outcrops in the Piceance Basin, Colorado, using three pyrolysis systems under conditions relevant to surface and in situ retorting approaches. Significant variations were observed in the shale oils, particularly the degree of conjugation of the constituent molecules and the distribution of nitrogen-containing compound classes. Comparison of FT-ICR MS results to other oil characteristics, such as specific gravity; saturate, aromatic, resin, asphaltene (SARA) distribution; and carbon number distribution determined by gas chromatography, indicated correspondence between higher average double bond equivalence (DBE) values and increasing asphaltene content. The results show that, based on the shale oil DBE distributions, highly conjugated species are enriched in samples produced under low pressure, high temperature conditions, and under high pressure, moderate temperature conditions in the presence of water. We also report, for the first time in any petroleum-like substance, the presence of N4 class compounds based on FT-ICR MS data. Using double bond equivalence and carbon number distributions, structures for the N4 class and other nitrogen-containing compounds are proposed.

Temperature-dependent phase-specific deformation mechanisms in a directionally solidified NiAl-Cr(Mo) lamellar composite

DOE PAGES

Yu, Dunji; An, Ke; Chen, Xu; ...

2015-10-09

Phase-specific thermal expansion and mechanical deformation behaviors of a directionally solidified NiAl–Cr(Mo) lamellar in situ composite were investigated by using real-time in situ neutron diffraction during compression at elevated temperatures up to 800 °C. Tensile and compressive thermal residual stresses were found to exist in the NiAl phase and Crss (solid solution) phase, respectively. Then, based on the evolution of lattice spacings and phase stresses, the phase-specific deformation behavior was analyzed qualitatively and quantitatively. Moreover, estimates of phase stresses were derived by Hooke's law on the basis of a simple method for the determination of stress-free lattice spacing in inmore » situ composites. During compressive loading, the NiAl phase yields earlier than the Crss phase. The Crss phase carries much higher stress than the NiAl phase, and displays consistent strain hardening at all temperatures. The NiAl phase exhibits strain hardening at relatively low temperatures and softening at high temperatures. During unloading, the NiAl phase yields in tension whereas the Crss phase unloads elastically. Additionally, post-test microstructural observations show phase-through cracks at room temperature, micro cracks along phase interfaces at 600 °C and intact lamellae kinks at 800 °C, which is due to the increasing deformability of both phases as temperature rises.« less

Temperature-dependent structure and phase variation of nickel silicide nanowire arrays prepared by in situ silicidation

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

Liu, Hailong; She, Guangwei, E-mail: shegw@mail.ipc.ac.cn; Mu, Lixuan

Graphical abstract: Display Omitted Highlight: ► Nickel silicides nanowire arrays prepared by a simple in situ silicidation method. ► Phases of nickel silicides could be varied by tuning the reaction temperature. ► A growth model was proposed for the nickel silicides nanowires. ► Diffusion rates of Ni and Si play a critical role for the phase variation. -- Abstract: In this paper, we report an in situ silicidizing method to prepare nickel silicide nanowire arrays with varied structures and phases. The in situ reaction (silicidation) between Si and NiCl{sub 2} led to conversion of Si nanowires to nickel silicide nanowires.more » Structures and phases of the obtained nickel silicides could be varied by changing the reaction temperature. At a relatively lower temperature of 700 °C, the products are Si/NiSi core/shell nanowires or NiSi nanowires, depending on the concentration of NiCl{sub 2} solution. At a higher temperature (800 °C and 900 °C), other phases of the nickel silicides, including Ni{sub 2}Si, Ni{sub 31}Si{sub 12}, and NiSi{sub 2}, were obtained. It is proposed that the different diffusion rates of Ni and Si atoms at different temperatures played a critical role in the formation of nickel silicide nanowires with different phases.« less

In situ optical measurements of Chang'E-3 landing site in Mare Imbrium: 2. Photometric properties of the regolith

NASA Astrophysics Data System (ADS)

Jin, Weidong; Zhang, Hao; Yuan, Ye; Yang, Yazhou; Shkuratov, Yuriy G.; Lucey, Paul G.; Kaydash, Vadim G.; Zhu, Meng-Hua; Xue, Bin; Di, Kaichang; Xu, Bin; Wan, Wenhui; Xiao, Long; Wang, Ziwei

2015-10-01

The panorama cameras onboard the Yutu Rover of the Chang'E-3 lunar mission acquired hundreds of high-resolution color images of the lunar surface and captured the first in situ lunar opposition effect (OE) since the Apollo era. We extracted the phase curve and the color ratio in three bands with the phase angle range from 2° to 141°. Photometric inversions using the Hapke model reveal that submicroscopic dusts are present in the landing area and both the coherent backscattering and the shadow hiding are responsible for the strong OE. Compared with spaceborne measurements, the grains in the landing site are brighter, more transparent, and appear to be better crystallized than the average maria basaltic grains. The results show that the phase-reddening effect appears to be present in the in situ phase curves. The current phase curve can be used as the ground-truth validations of any future spaceborne phase curve measurement over the landing site region.

Metastable tantalum oxide formation during the devitrification of amorphous tantalum thin films

DOE PAGES

Donaldson, Olivia K.; Hattar, Khalid; Trelewicz, Jason R.

2016-07-04

Microstructural evolution during the devitrification of amorphous tantalum thin films synthesized via pulsed laser deposition was investigated using in situ transmission electron microscopy (TEM) combined with ex situ isothermal annealing, bright-field imaging, and electron-diffraction analysis. The phases formed during crystallization and their stability were characterized as a function of the chamber pressure during deposition, devitrification temperature, and annealing time. A range of metastable nanocrystalline tantalum oxides were identified following devitrification including multiple orthorhombic oxide phases, which often were present with, or evolved to, the tetragonal TaO 2 phase. While the appearance of these phases indicated the films were evolving tomore » the stable form of tantalum oxide—monoclinic tantalum pentoxide—it was likely not achieved for the conditions considered due to an insufficient amount of oxygen present in the films following deposition. Nevertheless, the collective in situ and ex situ TEM analysis applied to thin film samples enabled the isolation of a number of metastable tantalum oxides. As a result, new insights were gained into the transformation sequence and stability of these nanocrystalline phases, which presents opportunities for the development of advanced tantalum oxide-based dielectric materials for novel memristor designs.« less

A study of suppressed formation of low-conductivity phases in doped Li 7La 3Zr 2O 12 garnets by in situ neutron diffraction

DOE PAGES

Chen, Yan; Rangasamy, Ezhiylmurugan; dela Cruz, Clarina R.; ...

2015-09-28

Doped Li 7La 3Zr 2O 12 garnets, oxide-based solids with good Li + conductivity and compatibility, show great potential as leading electrolyte material candidates for all-solid-state lithium ion batteries. Still yet, the conductive bulk usually suffers from the presence of secondary phases and the transition towards a low-conductivity tetragonal phase during synthesis. Dopants are designed to stabilize the high-conductive cubic phase and suppress the formation of the low-conductivity phases. In situ neutron diffraction enables a direct observation of the doping effects by monitoring the phase evolutions during garnet synthesis. It reveals the reaction mechanism involving the temporary presence of intermediatemore » phases. The off-stoichiometry due to the liquid Li 2CO 3 evaporation leads to the residual of the low-conductivity intermediate phase in the as-synthesized bulk. Appropriate doping of an active element may alter the component of the intermediate phases and promote the completion of the reaction. While the dopants aid to stabilize most of the cubic phase, a small amount of tetragonal phase tends to form under a diffusion process. Lastly, the in situ observations provide the guideline of process optimization to suppress the formation of unwanted low-conductivity phases.« less

Method of monitoring photoactive organic molecules in-situ during gas-phase deposition of the photoactive organic molecules

DOEpatents

Forrest, Stephen R.; Vartanian, Garen; Rolin, Cedric

2015-06-23

A method for in-situ monitoring of gas-phase photoactive organic molecules in real time while depositing a film of the photoactive organic molecules on a substrate in a processing chamber for depositing the film includes irradiating the gas-phase photoactive organic molecules in the processing chamber with a radiation from a radiation source in-situ while depositing the film of the one or more organic materials and measuring the intensity of the resulting photoluminescence emission from the organic material. One or more processing parameters associated with the deposition process can be determined from the photoluminescence intensity data in real time providing useful feedback on the deposition process.

Length-Scale-Dependent Phase Transformation of LiFePO4 : An In situ and Operando Study Using Micro-Raman Spectroscopy and XRD.

PubMed

Siddique, N A; Salehi, Amir; Wei, Zi; Liu, Dong; Sajjad, Syed D; Liu, Fuqiang

2015-08-03

The charge and discharge of lithium ion batteries are often accompanied by electrochemically driven phase-transformation processes. In this work, two in situ and operando methods, that is, micro-Raman spectroscopy and X-ray diffraction (XRD), have been combined to study the phase-transformation process in LiFePO4 at two distinct length scales, namely, particle-level scale (∼1 μm) and macroscopic scale (∼several cm). In situ Raman studies revealed a discrete mode of phase transformation at the particle level. Besides, the preferred electrochemical transport network, particularly the carbon content, was found to govern the sequence of phase transformation among particles. In contrast, at the macroscopic level, studies conducted at four different discharge rates showed a continuous but delayed phase transformation. These findings uncovered the intricate phase transformation in LiFePO4 and potentially offer valuable insights into optimizing the length-scale-dependent properties of battery materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Zhang, Kezhao; Ni, Longchang; Lei, Zhenglong, E-ma

The tensile deformation behavior of laser welded Ti{sub 2}AlNb joints was investigated using in situ analysis methods. The fracture mode of the single-B2-phase fusion zone was quasi-cleavage at room temperature and intergranular at 650 °C, while that of base metal was microvoid coalescence at both room temperature and 650 °C. Tensile deformation at room temperature was observed using in situ SEM tensile testing. In base metal, microcracks nucleated and propagated mainly within the O phase or along O/B2 phase boundaries. While both the cross- and multi-slips were found in the single-B2-phase fusion zone, a confocal laser scanning microscopy was usedmore » to observe the crack initiation and propagation process in situ at 650 °C. Cracks mainly formed along the B2/O phase boundaries in base metal, along the fragile grain boundaries of B2 phase in the fusion zone. The thermal simulation experiment and following TEM analysis indicated that the precipitation of continuous O-phase films along the B2 grain boundaries resulted in the high temperature brittleness of laser welded Ti{sub 2}AlNb joints. - Highlights: •Cracks formed within O phase or along B2/O boundaries in the base metal. •Cross- and multi-slips relieved stress in the fusion zone at room temperature. •Cracks mainly formed along the B2/O boundaries at 650 °C. •In the fusion zone, intergranular cracks were in situ observed at 650 °C. •O-phase films along B2 grain boundaries caused the high temperature brittleness.« less

Phase formation and strain relaxation of Ga2O3 on c-plane and a-plane sapphire substrates as studied by synchrotron-based x-ray diffraction

NASA Astrophysics Data System (ADS)

Cheng, Zongzhe; Hanke, Michael; Vogt, Patrick; Bierwagen, Oliver; Trampert, Achim

2017-10-01

Heteroepitaxial Ga2O3 was deposited on c-plane and a-plane oriented sapphire by plasma-assisted molecular beam epitaxy and probed by ex-situ and in-situ synchrotron-based x-ray diffraction. The investigation on c-plane sapphire determined a critical thickness of around 33 Å, at which the monoclinic β-phase forms on top of the hexagonal α-phase. A 143 Å thick single phase α-Ga2O3 was observed on a-plane sapphire, much thicker than the α-Ga2O3 on c-plane sapphire. The α-Ga2O3 relaxed very fast in the first 30 Å in both out-of-plane and in-plane directions as measured by the in-situ study.

Focusing on Fundamentals: A Reply to Koski and Horng

ERIC Educational Resources Information Center

Anzia, Sarah F.; Moe, Terry M.

2014-01-01

In this article, the authors Sarah A. Anzia and Terry M. Moe, offer a retort to William S. Koski and Elieen L. Horng's argument that their study of seniority-based transfer rules is narrow and that its findings only apply under limited circumstances. The Koski-Horng's study, by contrast, takes a broad frame--so broad that, as detailed in…

Purifying contaminated water

DOEpatents

Daughton, Christian G.

1983-01-01

Process for removing biorefractory compounds from contaminated water (e.g., oil shale retort waste-water) by contacting same with fragmented raw oil shale. Biorefractory removal is enhanced by preactivating the oil shale with at least one member of the group of carboxylic, acids, alcohols, aldehydes, ketones, ethers, amines, amides, sulfoxides, mixed ether-esters and nitriles. Further purification is obtained by stripping, followed by biodegradation and removal of the cells.

In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

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

Shen, Chenfei; Ge, Mingyuan; Luo, Langli

Here in this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li 15Si 4 phase while porous Si nanoparticles and nanowiresmore » transform to amorphous Li xSi phase, which is due to the effect of domain size on the stability of Li 15Si 4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.« less

In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

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

Shen, Chenfei; Ge, Mingyuan; Luo, Langli

In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphousmore » LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.« less

In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

NASA Astrophysics Data System (ADS)

Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

2016-08-01

In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.

In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

PubMed Central

Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

2016-01-01

In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires. PMID:27571919

In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

DOE PAGES

Shen, Chenfei; Ge, Mingyuan; Luo, Langli; ...

2016-08-30

Here in this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li 15Si 4 phase while porous Si nanoparticles and nanowiresmore » transform to amorphous Li xSi phase, which is due to the effect of domain size on the stability of Li 15Si 4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.« less

Mechanical properties of in situ consolidated nanocrystalline multi-phase Al-Pb-W alloy studied by nanoindentation

NASA Astrophysics Data System (ADS)

Varam, Sreedevi; Prasad, Muvva D.; Rao, K. Bhanu Sankara; Rajulapati, Koteswararao V.

2016-12-01

Formation of chunks of various sizes ranging between 2 and 6 mm was achieved using high-energy ball milling in Al-1at.%Pb-1at.%W alloy system at room temperature during milling itself, aiding in in situ consolidation. X-ray diffraction and transmission electron microscopy (TEM) studies indicate the formation of multi-phase structure with nanocrystalline structural features. From TEM data, an average grain size of 23 nm was obtained for Al matrix and the second-phase particles were around 5 nm. A high strain rate sensitivity (SRS) of 0.071 ± 0.004 and an activation volume of 4.71b3 were measured using nanoindentation. Modulus mapping studies were carried out using Berkovich tip in dynamic mechanical analysis mode coupled with in situ scanning probe microscopy imaging. The salient feature of this investigation is highlighting the role of different phases, their crystal structures and the resultant interfaces on the overall SRS and activation volume of a multi-phase nc material.

Variable Temperature Nuclear Magnetic Resonance and Magnetic Resonance Imaging System as a Novel Technique for In Situ Monitoring of Food Phase Transition.

PubMed

Song, Yukun; Cheng, Shasha; Wang, Huihui; Zhu, Bei-Wei; Zhou, Dayong; Yang, Peiqiang; Tan, Mingqian

2018-01-24

A nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) system with a 45 mm variable temperature (VT) sample probe (VT-NMR-MRI) was developed as an innovative technique for in situ monitoring of food phase transition. The system was designed to allow for dual deployment in either a freezing (-37 °C) or high temperature (150 °C) environment. The major breakthrough of the developed VT-NMR-MRI system is that it is able to measure the water states simultaneously in situ during food processing. The performance of the VT-NMR-MRI system was evaluated by measuring the phase transition for salmon flesh and hen egg samples. The NMR relaxometry results demonstrated that the freezing point of salmon flesh was -8.08 °C, and the salmon flesh denaturation temperature was 42.16 °C. The protein denaturation of egg was 70.61 °C, and the protein denaturation occurred at 24.12 min. Meanwhile, the use of MRI in phase transition of food was also investigated to gain internal structural information. All these results showed that the VT-NMR-MRI system provided an effective means for in situ monitoring of phase transition in food processing.

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

DOE PAGES

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro; ...

2018-06-12

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

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

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

The three phases of galaxy formation

NASA Astrophysics Data System (ADS)

Clauwens, Bart; Schaye, Joop; Franx, Marijn; Bower, Richard G.

2018-05-01

We investigate the origin of the Hubble sequence by analysing the evolution of the kinematic morphologies of central galaxies in the EAGLE cosmological simulation. By separating each galaxy into disc and spheroidal stellar components and tracing their evolution along the merger tree, we find that the morphology of galaxies follows a common evolutionary trend. We distinguish three phases of galaxy formation. These phases are determined primarily by mass, rather than redshift. For M* ≲ 109.5M⊙ galaxies grow in a disorganised way, resulting in a morphology that is dominated by random stellar motions. This phase is dominated by in-situ star formation, partly triggered by mergers. In the mass range 109.5M⊙ ≲ M* ≲ 1010.5M⊙ galaxies evolve towards a disc-dominated morphology, driven by in-situ star formation. The central spheroid (i.e. the bulge) at z = 0 consists mostly of stars that formed in-situ, yet the formation of the bulge is to a large degree associated with mergers. Finally, at M* ≳ 1010.5M⊙ growth through in-situ star formation slows down considerably and galaxies transform towards a more spheroidal morphology. This transformation is driven more by the buildup of spheroids than by the destruction of discs. Spheroid formation in these galaxies happens mostly by accretion at large radii of stars formed ex-situ (i.e. the halo rather than the bulge).

Field-induced polarization rotation and phase transitions in 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 piezoceramics observed by in situ high-energy x-ray scattering

NASA Astrophysics Data System (ADS)

Hou, Dong; Usher, Tedi-Marie; Fulanovic, Lovro; Vrabelj, Marko; Otonicar, Mojca; Ursic, Hana; Malic, Barbara; Levin, Igor; Jones, Jacob L.

2018-06-01

Changes to the crystal structure of 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic C m at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF results show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. This study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-x PT piezoceramics.

Rapid Retort Processing of Eggs

DTIC Science & Technology

2006-12-04

cyclodextrin, xanthan gum , ι-carrageenan, λ-carrageenan, κ-carrageenan, guar gum , locust bean gum , xanthan gum and starch. To improve the flavor of the...Cyclodextrin and κ-carrageenan were not effective in preventing synerisis. Guar gum and locust bean gum , and λ-carrageenan resulted in products with a slimy...Laboratory batches were prepared by hydrating the xanthan gum and pregelatinized starch in water which contained the salt and citric acid. The powdered

Purifying contaminated water. [DOE patent application

DOEpatents

Daughton, C.G.

1981-10-27

Process is presented for removing biorefactory compounds from contaminated water (e.g., oil shale retort waste-water) by contacting same with fragmented raw oil shale. Biorefractory removal is enhanced by preactivating the oil shale with at least one member of the group of carboxylic acids, alcohols, aldehydes, ketones, ethers, amines, amides, sulfoxides, mixed ether-esters and nitriles. Further purification is obtained by stripping, followed by biodegradation and removal of the cells.

Rapid Assembly Module for Traypacks

DTIC Science & Technology

2006-01-01

napkins , trays, utensils, garbage bags, etc. Food items will be dry, canned, or other retorted goods that are shelf-stable and require no...marked on the floor of the container with ink . When an alternative configuration is selected, a new manual will be issued by the PI. The revised manual...50 solders one meal. Accessories will include such items as cups, napkins , trays, utensils, garbage bags, etc. Food items will be dry, canned, or

Construction and use of an inexpensive "anthropometer".

PubMed

Clarke, G S

1996-08-01

An inexpensive anthropometer, suitable for use in undergraduate projects, was constructed from aluminum rod and components designed from laboratory retort stands. Only modest workshop skills and widely available machine tools were required to produce the device, which could be used to take accurate and reproducible measurements of linear dimensions and the angles of orientation of body segments. Its use in student projects indicates the value of the angular measurements in investigating posture.

Size fractionation in mercury-bearing airborne particles (HgPM 10) at Almadén, Spain: Implications for inhalation hazards around old mines

NASA Astrophysics Data System (ADS)

Moreno, Teresa; Higueras, Pablo; Jones, Tim; McDonald, Iain; Gibbons, Wes

Almadén has a >2000y mining history and an unprecedented legacy of mercury contamination. Resuspended airborne particles were extracted from mine waste (Las Cuevas), retort site soil (Almadenejos), and urban car park dust (Almadén), separated into fine (PM 10) and coarse (PM >10 μm ) fractions, analysed for mercury using ICP-MS, and individual HgPM characterised using SEM. Cold extractable mercury concentrations in PM 10 range from 100 to 150 μg g -1 (car parks), to nearly 6000 μg g -1 (mine waste), reaching a world record of 95,000 μg g -1 above the abandoned retort at Almadenejos where ultrafine HgPM have pervaded the brickwork and soil and entered the food chain: edible wild asparagus stem material from here contains 35-65 μg g -1 Hg, and pig hair from animals living, inhaling and ingesting HgPM 10 at the site yielded 8-10 μg g -1. The PM 10 fraction (dusts easily wind transported and deeply inhaled) contains much more mercury than the coarser fraction. The contribution of HgPM 10 to ecosystem contamination and potential human health effects around old mercury mines has been underestimated.

Nucleation of Iron Oxide Nanoparticles Mediated by Mms6 Protein in Situ

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

Kashyap, Sanjay; Woehl, Taylor J; Liu, Xunpei

2014-09-23

Biomineralization proteins are widely used as templating agents in biomimetic synthesis of a variety of organic–inorganic nanostructures. However, the role of the protein in controlling the nucleation and growth of biomimetic particles is not well understood, because the mechanism of the bioinspired reaction is often deduced from ex situ analysis of the resultant nanoscale mineral phase. Here we report the direct visualization of biomimetic iron oxide nanoparticle nucleation mediated by an acidic bacterial recombinant protein, Mms6, during an in situ reaction induced by the controlled addition of sodium hydroxide to solution-phase Mms6 protein micelles incubated with ferric chloride. Using inmore » situ liquid cell scanning transmission electron microscopy we observe the liquid iron prenucleation phase and nascent amorphous nanoparticles forming preferentially on the surface of protein micelles. Our results provide insight into the early steps of protein-mediated biomimetic nucleation of iron oxide and point to the importance of an extended protein surface during nanoparticle formation.« less

In-column bonded phase polymerization for improved packing uniformity

PubMed Central

Huckabee, Alexis G.; Yerneni, Charu; Jacobson, Rachel E.; Alzate, Edwin J.; Chen, Tse-Hong; Wirth, Mary J.

2017-01-01

It is difficult to pack chromatographic particles having polymeric-bonded phases because solvents used for making a stable slurry cause the polymer layer to swell. Growth of the polymer inside the column (in situ) after packing was investigated and compared with conventional, ex situ polymer growth. The method of activators generated by electron transfer, along with atom-transfer radical polymerization, enabled polymerization under ambient conditions. Nonporous, 0.62 µm silica particles with silane initiators were used. Polyacrylamide films with a hydrated thickness of 23 nm in 75:25 water/isopropanol grew in 55 min for both in situ and ex situ preparations, and the same carbon coverage was observed. Higher chromatographic resolution and better column-to-column reproducibility were observed for in situ polymer growth, as evaluated by hydrophilic interaction liquid chromatography for the model glycoprotein, ribonuclease B. In situ polymer growth was also found to give lower eddy diffusion, as shown by a narrower peak width for injected acetonitrile in 50:50 acetonitrile/water. When columns were packed more loosely, bed collapse occurred quickly for ex situ, but not for in situ, polymer growth. The higher resolution and stability for in situ polymer growth is explained by packing with hard, rather than soft, contacts between particles. PMID:28387037

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

PubMed

Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

NASA Astrophysics Data System (ADS)

Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques

DOE PAGES

Durham, Jessica L.; Brady, Alexander B.; Cama, Christina A.; ...

2017-08-02

Here, the structure of pristine AgFeO 2 and phase makeup of Ag 0.2FeO1.6 (a one-pot composite comprised of nanocrystalline stoichiometric AgFeO 2 and amorphous γ-Fe 2O 3 phases) was investigated using synchrotron x-ray diffraction. A new stacking-fault model was proposed for AgFeO2 powder synthesized using the co-precipitation method. The lithiation/de-lithiation mechanisms of silver ferrite, AgFeO 2 and Ag 0.2FeO 1.6 were investigated using ex-situ, in-situ, and operando characterization techniques. An amorphous γ-Fe 2O 3 component in the Ag 0.2FeO 1.6 sample is quantified. Operando XRD of electrochemically reduced AgFeO 2 and Ag 0.2FeO 1.6 composites demonstrated differences in the structuralmore » evolution of the nanocrystalline AgFeO 2 component. As complimentary techniques to XRD, ex-situ x-ray Absorption Spectroscopy (XAS) provided insight into the short-range structure of the (de)lithiated nanocrystalline electrodes, and a novel in-situ high energy x-ray fluorescence nanoprobe (HXN) mapping measurement was applied to spatially resolve the progression of discharge. Based on the results, a redox mechanism is proposed where the full reduction of Ag + to Ag0 and partial reduction of Fe 3+ to Fe 2+ occur on reduction to 1.0 V, resulting in a Li 1+yFe IIIFe IIyO 2 phase. The Li 1+yFe IIIFe IIyO 2 phase can then reversibly cycle between Fe 3+ and Fe 2+ oxidation states, permitting good capacity retention over 50 cycles. In the Ag 0.2FeO 1.6 composite, a substantial amorphous γ-Fe 2O 3 component is observed which discharges to rock salt LiFe 2O 3 and Fe 0 metal phase in the 3.5 – 1.0 V voltage range (in parallel with the AgFeO 2 mechanism), and reversibly reoxidizes to a nanocrystalline iron oxide phase.« less

Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques

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

Durham, Jessica L.; Brady, Alexander B.; Cama, Christina A.

Here, the structure of pristine AgFeO 2 and phase makeup of Ag 0.2FeO1.6 (a one-pot composite comprised of nanocrystalline stoichiometric AgFeO 2 and amorphous γ-Fe 2O 3 phases) was investigated using synchrotron x-ray diffraction. A new stacking-fault model was proposed for AgFeO2 powder synthesized using the co-precipitation method. The lithiation/de-lithiation mechanisms of silver ferrite, AgFeO 2 and Ag 0.2FeO 1.6 were investigated using ex-situ, in-situ, and operando characterization techniques. An amorphous γ-Fe 2O 3 component in the Ag 0.2FeO 1.6 sample is quantified. Operando XRD of electrochemically reduced AgFeO 2 and Ag 0.2FeO 1.6 composites demonstrated differences in the structuralmore » evolution of the nanocrystalline AgFeO 2 component. As complimentary techniques to XRD, ex-situ x-ray Absorption Spectroscopy (XAS) provided insight into the short-range structure of the (de)lithiated nanocrystalline electrodes, and a novel in-situ high energy x-ray fluorescence nanoprobe (HXN) mapping measurement was applied to spatially resolve the progression of discharge. Based on the results, a redox mechanism is proposed where the full reduction of Ag + to Ag0 and partial reduction of Fe 3+ to Fe 2+ occur on reduction to 1.0 V, resulting in a Li 1+yFe IIIFe IIyO 2 phase. The Li 1+yFe IIIFe IIyO 2 phase can then reversibly cycle between Fe 3+ and Fe 2+ oxidation states, permitting good capacity retention over 50 cycles. In the Ag 0.2FeO 1.6 composite, a substantial amorphous γ-Fe 2O 3 component is observed which discharges to rock salt LiFe 2O 3 and Fe 0 metal phase in the 3.5 – 1.0 V voltage range (in parallel with the AgFeO 2 mechanism), and reversibly reoxidizes to a nanocrystalline iron oxide phase.« less

Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques.

PubMed

Durham, Jessica L; Brady, Alexander B; Cama, Christina A; Bock, David C; Pelliccione, Christopher J; Zhang, Qing; Ge, Mingyuan; Li, Yue Ru; Zhang, Yiman; Yan, Hanfei; Huang, Xiaojing; Chu, Yong; Takeuchi, Esther S; Takeuchi, Kenneth J; Marschilok, Amy C

2017-08-23

The structure of pristine AgFeO 2 and phase makeup of Ag 0.2 FeO 1.6 (a one-pot composite comprised of nanocrystalline stoichiometric AgFeO 2 and amorphous γ-Fe 2 O 3 phases) was investigated using synchrotron X-ray diffraction. A new stacking-fault model was proposed for AgFeO 2 powder synthesized using the co-precipitation method. The lithiation/de-lithiation mechanisms of silver ferrite, AgFeO 2 and Ag 0.2 FeO 1.6 were investigated using ex situ, in situ, and operando characterization techniques. An amorphous γ-Fe 2 O 3 component in the Ag 0.2 FeO 1.6 sample is quantified. Operando XRD of electrochemically reduced AgFeO 2 and Ag 0.2 FeO 1.6 composites demonstrated differences in the structural evolution of the nanocrystalline AgFeO 2 component. As complimentary techniques to XRD, ex situ X-ray Absorption Spectroscopy (XAS) provided insight into the short-range structure of the (de)lithiated nanocrystalline electrodes, and a novel in situ high energy X-ray fluorescence nanoprobe (HXN) mapping measurement was applied to spatially resolve the progression of discharge. Based on the results, a redox mechanism is proposed where the full reduction of Ag + to Ag 0 and partial reduction of Fe 3+ to Fe 2+ occur on reduction to 1.0 V, resulting in a Li 1+y Fe III Fe II y O 2 phase. The Li 1+y Fe III Fe II y O 2 phase can then reversibly cycle between Fe 3+ and Fe 2+ oxidation states, permitting good capacity retention over 50 cycles. In the Ag 0.2 FeO 1.6 composite, a substantial amorphous γ-Fe 2 O 3 component is observed which discharges to rock salt LiFe 2 O 3 and Fe 0 metal phase in the 3.5-1.0 V voltage range (in parallel with the AgFeO 2 mechanism), and reversibly reoxidizes to a nanocrystalline iron oxide phase.

High-resolution mass spectrometry of nitrogenous compounds of the Colorado Green River formation oil shale.

NASA Technical Reports Server (NTRS)

Simoneit, B. R.; Schnoes, H. K.; Haug, P.; Burlingame, A. L.

1971-01-01

Basic nitrogenous compounds isolated from extracts of Green River Formation oil shale were analyzed. The major homologous constituents found were the compositional types - namely, quinolines, tetrahydrequinolines with minor amounts of pyridines and indoles series and traces of more aromatized nitrogen compounds. These results are correlated with nitrogen compounds isolated from Green River Formation retort oil and are a survey of the unaltered nitrogen compounds indigeneous to the shale.

Retort braze bonding of borsic/aluminum composite sheet to titanium

NASA Technical Reports Server (NTRS)

Webb, B. A.; Dolowy, J. F., Jr.

1975-01-01

Braze bonding studies between Borsic/aluminum composite and titanium sheet were conducted to establish acceptable brazing techniques and to assess potential joint efficiencies. Excellent braze joints were produced which exhibited joint strengths exceeding 117 MPa (17,000 psi) and which retained up to 2/3 of this strength at 589 K (600 F). Noticeable composite strength degradation resulting from the required high temperature braze cycle was found to be a problem.

6. VIEW LOOKING NORTHWEST FROM THE IMAGE LEFT TO THE ...

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

6. VIEW LOOKING NORTHWEST FROM THE IMAGE LEFT TO THE IMAGE RIGHT IS THE CHARCOAL HOUSE, THE RETORT SHED IN THE BACKGROUND, THE MILL ANNEX, THE MACHINE SHOP, AND THE ELECTRIC MOTOR ROOM. THE MILL BUILDING IS IN THE BACKGROUND CENTER RIGHT AND ONE OF THE ORE DELIVERY TRESTLES EXTENDING FROM THE MILL BUILDING TO RIGHT IMAGE EDGE. - Standard Gold Mill, East of Bodie Creek, Northeast of Bodie, Bodie, Mono County, CA

Metastable and equilibrium phase formation in sputter-deposited Ti/Al multilayer thin films

NASA Astrophysics Data System (ADS)

Lucadamo, G.; Barmak, K.; Lavoie, C.; Cabral, C., Jr.; Michaelsen, C.

2002-06-01

The sequence and kinetics of metastable and equilibrium phase formation in sputter deposited multilayer thin films was investigated by combining in situ synchrotron x-ray diffraction (XRD) with ex situ electron diffraction and differential scanning calorimetry (DSC). The sequence included both cubic and tetragonal modifications of the equilibrium TiAl3 crystal structure. Values for the formation activation energies of the various phases in the sequence were determined using the XRD and DSC data obtained here, as well as activation energy data reported in the literature.

In Situ Clay Formation: Evaluation of a Proposed New Technology for Stable Containment Barriers

DTIC Science & Technology

2004-03-01

situ layered double hydroxide precipitation........... 23 4.2.1 Solution preparation and column mixing...22 Table 4.2 Summary of in situ precipitation of layered double hydroxide (LDH...effect on permeability for the smallest volume precipitated is sheet silicates or layered -clay phases (hereafter called “clays”). In natural

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

PubMed

Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

2016-11-24

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

Injectable CMC/PEI gel as an in vivo scaffold for demineralized bone matrix.

PubMed

Kim, Kyung Sook; Kang, Yun Mi; Lee, Ju Young; Kim, E Sle; Kim, Chun Ho; Min, Byoung Hyun; Lee, Hai Bang; Kim, Jae Ho; Kim, Moon Suk

2009-01-01

A number of materials have been considered as sources of grafts to repair bone defects. Here, we examined the possibility of creating in situ-forming gels from sodium carboxymethylcellulose (CMC) and poly(ethyleneimine) (PEI) for use as an in vivo carrier of demineralized bone matrix (DBM). The interaction between anionic CMC and cationic PEI was examined by evaluating phase transition behavior and viscosity of CMC solutions containing 0-30 wt% PEI. CMC solutions containing 10 wt% PEI exhibited a sol-to-gel phase transition at temperatures greater than 35 degrees C. The phase transition is caused by electrostatic crosslinking of the CMC/PEI solution to form a gel with a three-dimensional network structure. In situ-formed gel implants were successfully fabricated in vivo by simple subcutaneous injection of the CMC/PEI (90/10) solution (with and without DBM) into Fisher rats. The resulting in situ-formed implant maintained its shape for 28 days in vitro and in vivo. Our results show that in situ-forming CMC/PEI gels can serve as a DBM carrier that can be delivered with a minimally invasive procedure.

In situ REM and ex situ SPM studies of silicon (111) surface

NASA Astrophysics Data System (ADS)

Aseev, A. L.; Kosolobov, S. S.; Latyshev, A. V.; Song, Se Ahn; Saranin, A. A.; Zotov, A. V.; Lifshits, V. G.

2005-09-01

Combination of experimental methods, including ultrahigh vacuum in situ reflection electron microscopy, scanning tunnelling microscopy and atomic force microscopy, has been applied for analysis of surface structure and dynamic processes on silicon (111) surfaces during sublimation, rapid temperature cooling, oxygen reactions and metal-silicon surface phase formation. From analysis of triangular negative islands, 0.08 nm in depth, which were forming during quenching, it was deduced the effective activation energy of the island generation is equalled to 0.35 eV and made conclusion that the (1 × 1) (7 × 7) phase transition on Si(111) assumes to be responsible for the negative island nucleation. On the base of the in situ REM study, the dependence of step motion, initiated by surface vacancies generation during oxygen-silicon interaction, on the terrace width was measured. Peculiarities of the initial stages of silicon surface oxidation at low pressures were considered. From precision measurements, the top silicon atom density was determined for the metal-silicon surface phase formed during Na, Ca, Mg and Ag deposition on clean silicon (111) surface.

Test plan for Geo-Cleanse{reg_sign} demonstration (in situ destruction of dense non-aqueous phase liquid (DNAPL))

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

Jerome, K.M.; Looney, B.B.; Accorsi, F.

1996-09-01

Soils and groundwater beneath an abandoned process sewer line in the A/M Area of the Savannah River Site (SRS) contain elevated levels of volatile organic compounds, specifically trichloroethylene (TCE) and tetrachloroethylene (PCE), two common chlorinated solvents. These compounds have low aqueous solubilities, thus when released to the subsurface in sufficient quantity, tend to exist as immiscible fluids or nonaqueous phase liquids (NAPLs). Because chlorinated solvents are also denser than water, they are referred to by the acronym DNAPLs, or dense non-aqueous phase liquids. Technologies targeted at the efficient characterization or removal of DNAPL are not currently proven. For example, mostmore » DNAPL studies rely on traditional soil and water sampling and the fortuitous observation of immiscible solvent. Once DNAPL is identified, soil excavation (which is only applicable to small contained spill sites) is the only proven cleanup method. New cleanup approaches based on destruction of DNAPL either in situ or ex situ have been proposed and tested at the pilot scale. The proposed demonstration, as described in this report will evaluate the applicability to DNAPL plumes of a technology proven for in situ destruction of light non-aqueous phase liquids (LNAPLs) such as oils.« less

Kinetics of methane hydrate replacement with carbon dioxide and nitrogen gas mixture using in situ NMR spectroscopy.

PubMed

Cha, Minjun; Shin, Kyuchul; Lee, Huen; Moudrakovski, Igor L; Ripmeester, John A; Seo, Yutaek

2015-02-03

In this study, the kinetics of methane replacement with carbon dioxide and nitrogen gas in methane gas hydrate prepared in porous silica gel matrices has been studied by in situ (1)H and (13)C NMR spectroscopy. The replacement process was monitored by in situ (1)H NMR spectra, where about 42 mol % of the methane in the hydrate cages was replaced in 65 h. Large amounts of free water were not observed during the replacement process, indicating a spontaneous replacement reaction upon exposing methane hydrate to carbon dioxide and nitrogen gas mixture. From in situ (13)C NMR spectra, we confirmed that the replacement ratio was slightly higher in small cages, but due to the composition of structure I hydrate, the amount of methane evolved from the large cages was larger than that of the small cages. Compositional analysis of vapor and hydrate phases was also carried out after the replacement reaction ceased. Notably, the composition changes in hydrate phases after the replacement reaction would be affected by the difference in the chemical potential between the vapor phase and hydrate surface rather than a pore size effect. These results suggest that the replacement technique provides methane recovery as well as stabilization of the resulting carbon dioxide hydrate phase without melting.

Understanding the phase formation kinetics of nano-crystalline kesterite deposited on mesoscopic scaffolds via in situ multi-wavelength Raman-monitored annealing.

PubMed

Wang, Zhuoran; Elouatik, Samir; Demopoulos, George P

2016-10-26

Kesterite, a highly promising photo-absorbing crystalline form of Cu 2 ZnSnS 4 (CZTS), has been prepared via various routes. However, the lack of in-depth understanding of the dynamic phase formation process of kesterite leads to difficulties in optimizing its annealing conditions, hence its light harvesting performance. In this paper, in situ Raman monitored-annealing is applied to study the phase formation kinetics of nano-crystalline kesterite from a precursor deposited on a TiO 2 mesoscopic scaffold. By performing in situ Raman annealing under different experimental conditions and wavelengths, several facts have been discovered: kesterite crystallization starts at as low as 170 °C, but after short time annealing at 300 °C followed by cooling, the initially formed kesterite is found to decompose. Annealing at 400 °C or higher is proven to be sufficient for stabilizing the kesterite phase. Annealing at the higher temperature of 500 °C is necessary though to promote a complete reaction and thus eliminate the parasitic copper tin sulfide (CTS) impurity intermediates identified at lower annealing temperatures. More importantly, the real-time temperature dependence of Raman peak intensity enhancement, shift and broadening for CZTS is established experimentally at 500 °C for 1 h, providing a valuable reference in future CZTS research. This work demonstrates the significance of using in situ Raman spectroscopy in elucidating the kesterite phase formation kinetics, a critical step towards full crystal phase control - a prerequisite for developing fully functional CZTS-based optoelectronic devices.

Ferroelastic domain structure and phase transition in single-crystalline [PbZn 1/3Nb 2/3O 3] 1-x[PbTiO 3] x observed via in situ x-ray microbeam

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

Li, Tao; Du, Zehui; Tamura, Nobumichi

(1-x)Pb(Zn 1/3Nb 2/3)O 3-xPbTiO 3 ((1-x)PZN-xPT in short) is one of the most important piezoelectric materials. In this study, we extensively investigated (1-x)PZN-xPT (x = 0.07–0.11) ferroelectric single crystals using in-situ synchrotron μXRD, complemented by TEM and PFM, to correlate microstructures with phase transitions. The results reveal that (i) at 25°C, the equilibrium state of (1-x)PZN-xPT is a metastable orthorhombic phase for x = 0.07 and 0.08, while it shows coexistence of orthorhombic and tetragonal phases for x = 0.09 and x = 0.11, with all ferroelectric phases accompanied by ferroelastic domains; (ii) upon heating, the phase transformation in xmore » = 0.07 is Orthorhombic → Monoclinic → Tetragonal → Cubic. The coexistence of ferroelectric tetragonal and paraelectric cubic phases was in-situ observed in x = 0.08 above Curie temperature (T C), and (iii) phase transition can be explained by the evolution of the ferroelectric and ferroelastic domains. These results disclose that (1-x)PZN-xPT are in an unstable regime, which is possible factor for its anomalous dielectric response and high piezoelectric coefficient.« less

Ferroelastic domain structure and phase transition in single-crystalline [PbZn 1/3Nb 2/3O 3] 1-x[PbTiO 3] x observed via in situ x-ray microbeam

DOE PAGES

Li, Tao; Du, Zehui; Tamura, Nobumichi; ...

2017-11-10

(1-x)Pb(Zn 1/3Nb 2/3)O 3-xPbTiO 3 ((1-x)PZN-xPT in short) is one of the most important piezoelectric materials. In this study, we extensively investigated (1-x)PZN-xPT (x = 0.07–0.11) ferroelectric single crystals using in-situ synchrotron μXRD, complemented by TEM and PFM, to correlate microstructures with phase transitions. The results reveal that (i) at 25°C, the equilibrium state of (1-x)PZN-xPT is a metastable orthorhombic phase for x = 0.07 and 0.08, while it shows coexistence of orthorhombic and tetragonal phases for x = 0.09 and x = 0.11, with all ferroelectric phases accompanied by ferroelastic domains; (ii) upon heating, the phase transformation in xmore » = 0.07 is Orthorhombic → Monoclinic → Tetragonal → Cubic. The coexistence of ferroelectric tetragonal and paraelectric cubic phases was in-situ observed in x = 0.08 above Curie temperature (T C), and (iii) phase transition can be explained by the evolution of the ferroelectric and ferroelastic domains. These results disclose that (1-x)PZN-xPT are in an unstable regime, which is possible factor for its anomalous dielectric response and high piezoelectric coefficient.« less

In Situ Thermal Treatment of Chlorinated Solvents: Fundamentals and Field Applications

EPA Pesticide Factsheets

This report contains information about the use of in situ thermal treatment technologies to treat chlorinated solvents in source zones containing free-phase contamination or high concentrations of contaminants.

Emissions and Char Quality of Flame-Curtain "Kon Tiki" Kilns for Farmer-Scale Charcoal/Biochar Production.

PubMed

Cornelissen, Gerard; Pandit, Naba Raj; Taylor, Paul; Pandit, Bishnu Hari; Sparrevik, Magnus; Schmidt, Hans Peter

2016-01-01

Pyrolysis of organic waste or woody materials yields charcoal, a stable carbonaceous product that can be used for cooking or mixed into soil, in the latter case often termed "biochar". Traditional kiln technologies for charcoal production are slow and without treatment of the pyrolysis gases, resulting in emissions of gases (mainly methane and carbon monoxide) and aerosols that are both toxic and contribute to greenhouse gas emissions. In retort kilns pyrolysis gases are led back to a combustion chamber. This can reduce emissions substantially, but is costly and consumes a considerable amount of valuable ignition material such as wood during start-up. To overcome these problems, a novel type of technology, the Kon-Tiki flame curtain pyrolysis, is proposed. This technology combines the simplicity of the traditional kiln with the combustion of pyrolysis gases in the flame curtain (similar to retort kilns), also avoiding use of external fuel for start-up. A field study in Nepal using various feedstocks showed char yields of 22 ± 5% on a dry weight basis and 40 ± 11% on a C basis. Biochars with high C contents (76 ± 9%; n = 57), average surface areas (11 to 215 m2 g-1), low EPA16-PAHs (2.3 to 6.6 mg kg-1) and high CECs (43 to 217 cmolc/kg)(average for all feedstocks, mainly woody shrubs) were obtained, in compliance with the European Biochar Certificate (EBC). Mean emission factors for the flame curtain kilns were (g kg-1 biochar for all feedstocks); CO2 = 4300 ± 1700, CO = 54 ± 35, non-methane volatile organic compounds (NMVOC) = 6 ± 3, CH4 = 30 ± 60, aerosols (PM10) = 11 ± 15, total products of incomplete combustion (PIC) = 100 ± 83 and NOx = 0.4 ± 0.3. The flame curtain kilns emitted statistically significantly (p<0.05) lower amounts of CO, PIC and NOx than retort and traditional kilns, and higher amounts of CO2. With benefits such as high quality biochar, low emission, no need for start-up fuel, fast pyrolysis time and, importantly, easy and cheap construction and operation the flame curtain technology represent a promising possibility for sustainable rural biochar production.

Emissions and Char Quality of Flame-Curtain "Kon Tiki" Kilns for Farmer-Scale Charcoal/Biochar Production

PubMed Central

Cornelissen, Gerard; Pandit, Naba Raj; Taylor, Paul; Pandit, Bishnu Hari; Sparrevik, Magnus; Schmidt, Hans Peter

2016-01-01

Flame Curtain Biochar Kilns Pyrolysis of organic waste or woody materials yields charcoal, a stable carbonaceous product that can be used for cooking or mixed into soil, in the latter case often termed "biochar". Traditional kiln technologies for charcoal production are slow and without treatment of the pyrolysis gases, resulting in emissions of gases (mainly methane and carbon monoxide) and aerosols that are both toxic and contribute to greenhouse gas emissions. In retort kilns pyrolysis gases are led back to a combustion chamber. This can reduce emissions substantially, but is costly and consumes a considerable amount of valuable ignition material such as wood during start-up. To overcome these problems, a novel type of technology, the Kon-Tiki flame curtain pyrolysis, is proposed. This technology combines the simplicity of the traditional kiln with the combustion of pyrolysis gases in the flame curtain (similar to retort kilns), also avoiding use of external fuel for start-up. Biochar Characteristics A field study in Nepal using various feedstocks showed char yields of 22 ± 5% on a dry weight basis and 40 ± 11% on a C basis. Biochars with high C contents (76 ± 9%; n = 57), average surface areas (11 to 215 m2 g-1), low EPA16—PAHs (2.3 to 6.6 mg kg-1) and high CECs (43 to 217 cmolc/kg)(average for all feedstocks, mainly woody shrubs) were obtained, in compliance with the European Biochar Certificate (EBC). Gas Emission Factors Mean emission factors for the flame curtain kilns were (g kg-1 biochar for all feedstocks); CO2 = 4300 ± 1700, CO = 54 ± 35, non-methane volatile organic compounds (NMVOC) = 6 ± 3, CH4 = 30 ± 60, aerosols (PM10) = 11 ± 15, total products of incomplete combustion (PIC) = 100 ± 83 and NOx = 0.4 ± 0.3. The flame curtain kilns emitted statistically significantly (p<0.05) lower amounts of CO, PIC and NOx than retort and traditional kilns, and higher amounts of CO2. Implications With benefits such as high quality biochar, low emission, no need for start-up fuel, fast pyrolysis time and, importantly, easy and cheap construction and operation the flame curtain technology represent a promising possibility for sustainable rural biochar production. PMID:27191397

Integrating the Land and Air Components in an Anti-Access/Area Denial Environment

DTIC Science & Technology

2013-06-01

to his pursuit and bomber squadrons being already tasked to their limits, Fredendall retorted that he had lost 300 men due to enemy actions and the...190 Murray and Scales, The Iraq War, 173. 191 Author’s personal experience as a Close Air Support planner and Strike Package ...in the future the command and control structure will need to support air strike packages transitioning from interdiction and global strike missions to

Exploring Convergent Evolution to Provide a Foundation for Protein Engineering

DTIC Science & Technology

2009-02-26

information if it does not display a currently valid OMB control number PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ORGANIZATION. RETORT DATE (DD-MM-YYYY...the DivergentSet and MotifCluster Algorithms Using support from this grant, we developed two software packages that provide key infrastructure for...software package we developed, MotifCluster," provides a novel way of detecting distantly related homologs, one of the key aims of the proposal. Unlike

An Economic and Ecologic Comparison of the Nuclear Stimulation of Natural Gas Fields with Retorting of Oil Shale

DTIC Science & Technology

1975-06-06

the U.S. Atomic Energy Commission, and the Department of the Interior, with the Program Management provided by Geonuclear Corporation of Las Vegas...of native species. --Addition of irrigation water when initially planting. —Protection from access by herbivores. — Management after planting. No...physical conditions or water qaulity (temperature, pH, toxic substances) include trout and whitefish as well as the threatened species mentioned above

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew L.; Smith, Jesse; Sinogeikin, Stanislav

2017-12-01

We report real-time observations of a phase transition in the ionic solid CaF2 , a model A B2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Measurement of Body-Centered-Cubic Aluminum at 475 GPa [Observation of Body-Centered-Cubic Aluminum at 475 GPa

DOE PAGES

Polsin, D. N.; Fratanduono, D. E.; Rygg, J. R.; ...

2017-10-27

Nanosecond in situ x-ray diffraction and simultaneous velocimetry measurements were used to determine the crystal structure and pressure, respectively, of ramp compressed aluminum at stress states between 111 and 475 GPa. The solid-solid Al phase transformations, fcc-hcp and hcp-bcc, are observed at 216 ± 9 GPa and 321 ± 12 GPa, respectively, with the bcc phase persisting to 475 GPa. Here, this is the first in situ observation of the high-pressure bcc phase of Al. High-pressure texture of the hcp and bcc phases suggests close-packed or nearly close-packed lattice planes remain parallel through both transformations.

Measurement of Body-Centered-Cubic Aluminum at 475 GPa [Observation of Body-Centered-Cubic Aluminum at 475 GPa

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

Polsin, D. N.; Fratanduono, D. E.; Rygg, J. R.

Nanosecond in situ x-ray diffraction and simultaneous velocimetry measurements were used to determine the crystal structure and pressure, respectively, of ramp compressed aluminum at stress states between 111 and 475 GPa. The solid-solid Al phase transformations, fcc-hcp and hcp-bcc, are observed at 216 ± 9 GPa and 321 ± 12 GPa, respectively, with the bcc phase persisting to 475 GPa. Here, this is the first in situ observation of the high-pressure bcc phase of Al. High-pressure texture of the hcp and bcc phases suggests close-packed or nearly close-packed lattice planes remain parallel through both transformations.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

DOE PAGES

Kalita, Patricia E.; Specht, Paul Elliot; Root, Seth; ...

2017-12-21

Here, we report real-time observations of a phase transition in the ionic solid CaF 2, a model AB 2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Mercury speciation in the Mt. Amiata mining district (Italy): interplay between urban activities and mercury contamination

USGS Publications Warehouse

Rimondi, Valentina; Bardelli, Fabrizio; Benvenuti, Marco; Costagliola, Pilario; Gray, John E.; Lattanzi, Pierfranco

2014-01-01

A fundamental step to evaluate the biogeochemical and eco-toxicological significance of Hg dispersion in the environment is to determine speciation of Hg in solid matrices. In this study, several analytical techniques such as scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), sequential chemical extractions (SCEs), and X-ray absorption spectroscopy (XANES) were used to identify Hg compounds and Hg speciation in samples collected from the Mt. Amiata Hg mining district, southern Tuscany, Italy. Different geological materials, such as mine waste calcine (retorted ore), soil, stream sediment, and stream water suspended particulate matter were analyzed. Results show that the samples were generally composed of highly insoluble Hg compounds such as sulphides (HgS, cinnabar and metacinnabar), and more soluble Hg halides such as those associated with the mosesite group. Other moderately soluble Hg compounds, HgCl2, HgO and Hg0, were also identified in stream sediments draining the mining area. The presence of these minerals suggests active and continuous runoff of soluble Hg compounds from calcines, where such Hg compounds form during retorting, or later in secondary processes. Specifically, we suggest that, due to the proximity of Hg mines to the urban center of Abbadia San Salvatore, the influence of other anthropogenic activities was a key factor for Hg speciation, resulting in the formation of unusual Hg-minerals such as mosesite.

An in situ vapour phase hydrothermal surface doping approach for fabrication of high performance Co3O4 electrocatalysts with an exceptionally high S-doped active surface.

PubMed

Tan, Zhijin; Liu, Porun; Zhang, Haimin; Wang, Yun; Al-Mamun, Mohammad; Yang, Hua Gui; Wang, Dan; Tang, Zhiyong; Zhao, Huijun

2015-04-04

A facile in situ vapour phase hydrothermal (VPH) surface doping approach has been developed for fabrication of high performance S-doped Co3O4 electrocatalysts with an unprecedentedly high surface S content (>47%). The demonstrated VPH doping approach could be useful for enrichment of surface active sites for other metal oxide electrocatalysts.

Improved phase-ellipse method for in-situ geophone calibration.

USGS Publications Warehouse

Liu, Huaibao P.; Peselnick, L.

1986-01-01

For amplitude and phase response calibration of moving-coil electromagnetic geophones 2 parameters are needed, namely the geophone natural frequency, fo, and the geophone upper resonance frequency fu. The phase-ellipse method is commonly used for the in situ determination of these parameters. For a given signal-to-noise ratio, the precision of the measurement of fo and fu depends on the phase sensitivity, f(delta PHI/delta PHIf). For some commercial geophones (f(delta PHI/delta PHI) at fu can be an order of magnitude less than the sensitivity at fo. Presents an improved phase-ellipse method with increased precision. Compared to measurements made with the existing phase-ellipse methods, the method shows a 6- and 3-fold improvement in the precision, respectively, on measurements of fo and fu on a commercial geophone.-from Authors

Low temperature formation of higher-k cubic phase HfO{sub 2} by atomic layer deposition on GeO{sub x}/Ge structures fabricated by in-situ thermal oxidation

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

Zhang, R., E-mail: zhang@mosfet.t.u-tokyo.ac.jp; Department of Information Science and Electronic Engineering, Zhejiang University, 38 Zheda Road, Hangzhou 310027; Huang, P.-C.

2016-02-01

We have demonstrated a low temperature formation (300 °C) of higher-k HfO{sub 2} using atomic layer deposition (ALD) on an in-situ thermal oxidation GeO{sub x} interfacial layer. It is found that the cubic phase is dominant in the HfO{sub 2} film with an epitaxial-like growth behavior. The maximum permittivity of 42 is obtained for an ALD HfO{sub 2} film on a 1-nm-thick GeO{sub x} form by the in-situ thermal oxidation. It is suggested from physical analyses that the crystallization of cubic phase HfO{sub 2} can be induced by the formation of six-fold crystalline GeO{sub x} structures in the underlying GeO{sub x}more » interfacial layer.« less

The preparation of Zr-deuteride and phase stability studies of the Zr-D system

NASA Astrophysics Data System (ADS)

Maimaitiyili, T.; Steuwer, A.; Bjerkén, C.; Blomqvist, J.; Hoelzel, M.; Ion, J. C.; Zanellato, O.

2017-03-01

Deuteride phases in the zirconium-deuterium system in the temperature range 25-286 °C have been studied in-situ by high resolution neutron diffraction. The study primarily focused on observations of δ→γ transformation at 180 °C, and the peritectoid reaction α + δ ↔ γ at 255 °C in commercial grade Zr powder that was deuterated to a deuterium/Zr ratio of one to one. A detailed description of the zirconium deuteride preparation route by high temperature gas loading is also described. The lattice parameters of α-Zr, δ-ZrDx and ε-ZrDx were determined by whole pattern crystal structure analysis, using Rietveld and Pawley refinements, and are in good agreement with values reported in the literature. The controversial γ-hydride phase was observed both in-situ and ex-situ in deuterated Zr powder after a heat treatment at 286 °C and slow cooling.

In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

NASA Astrophysics Data System (ADS)

Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

2017-09-01

The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

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

Ouyang, Xin; Huang, Saifang; School of Materials Science and Technology, China University of Geosciences

2014-03-15

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to bemore » calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.« less

Structural properties of zirconia - in-situ high temperature XRD characterization

NASA Astrophysics Data System (ADS)

Kurpaska, Lukasz

2018-07-01

In this work, the effect of high temperature on structural properties of pure zirconium have been investigated. In-situ X-ray diffraction analysis of the oxide layer formed at temperature window 25-600 °C on pure zirconium were performed. Conducted experiment aimed at investigation of the zirconia phases developed on surface of the metallic substrate. Based on the conducted studies, possible stress state (during heating, continuous oxidation and cooling), cell parameters and HWHM factor were analyzed. A tetragonal and monoclinic phases peak shifts and intensities change were observed, suggesting that different phases react in different way upon temperature effect.

In meso in situ serial X-ray crystallography of soluble and membrane proteins

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

Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee

A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins,more » including the β{sub 2}-adrenoreceptor–G{sub s} protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development.« less

Towards 3D crystal orientation reconstruction using automated crystal orientation mapping transmission electron microscopy (ACOM-TEM).

PubMed

Kobler, Aaron; Kübel, Christian

2018-01-01

To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.

Microstructural Control via Copious Nucleation Manipulated by In Situ Formed Nucleants: Large-Sized and Ductile Metallic Glass Composites.

PubMed

Song, Wenli; Wu, Yuan; Wang, Hui; Liu, Xiongjun; Chen, Houwen; Guo, Zhenxi; Lu, Zhaoping

2016-10-01

A novel strategy to control the precipitation behavior of the austenitic phase, and to obtain large-sized, transformation-induced, plasticity-reinforced bulk metallic glass matrix composites, with good tensile properties, is proposed. By inducing heterogeneous nucleation of the transformable reinforcement via potent nucleants formed in situ, the characteristics of the austenitic phase are well manipulated. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-convergent ordering and displacive phase transition in pigeonite: in situ HT XRD study

NASA Astrophysics Data System (ADS)

Cámara, F.; Carpenter, M. A.; Domeneghetti, M. C.; Tazzoli, V.

A natural Ca-rich pigeonite (En47Fs43Wo10), free of augite exsolution products, was studied by in situ high-temperature single-crystal X-ray diffraction. The sample, monoclinic P21/c (a=9.719(7) Å, b=8.947(9) Å, c=5.251(3) Å, β=108.49(5), V=433.0(6) Å3), was annealed up to 1000 °C to induce a phase transition from P21/c to C2/c symmetry. Complete single-crystal X-ray diffraction data collections were carried out in situ at 650, 750, 850 and 950 °C after the crystal had reached equilibrium for the Fe-Mg intracrystalline exchange reaction at each temperature. The variation, with increasing temperature, of lattice parameters, of intensity of hkl reflections with h + k=2n + 1 (which vanish at high temperature) and of some geometrical parameters from structure refinement, showed that the displacive phase transition P21/cC2/c was continuous in character. This contrasts with the first-order character for the HT phase transition in pigeonite containing significantly less calcium.

Ion Implantation with in-situ Patterning for IBC Solar Cells

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

Graff, John W.

2014-10-24

Interdigitated back-side Contact (IBC) solar cells are the highest efficiency silicon solar cells currently on the market. Unfortunately the cost to produce these solar cells is also very high, due to the large number of processing steps required. Varian believes that only the combination of high efficiency and low cost can meet the stated goal of $1/Wp. The core of this program has been to develop an in-situ patterning capability for an ion implantation system capable of producing patterned doped regions for IBC solar cells. Such a patterning capable ion implanter can reduce the number of process steps required tomore » manufacture IBC cells, and therefore significantly reduce the cost. The present program was organized into three phases. Phase I was to select a patterning approach and determine the patterning requirements for IBC cells. Phase II consists of construction of a Beta ion implantation system containing in-situ patterning capability. Phase III consists of shipping and installation of the ion implant system in a customer factory where it will be tested and proven in a pilot production line.« less

In Situ XAS and XRD Studies of Substituted Spinel Lithium Manganese Oxides in the 4-5 V Region

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

McBreen, J.; Mukerjee, S.; Yang, X. Q.

Partial substitution of Mn in lithium manganese oxide spinel materials by Cu and Ni greatly affects the electrochemistry and the phase behavior of the cathode. Substitution with either metal or with a combination of both shortens the 4.2 V plateau and results in higher voltage plateaus. In situ x-ray absorption (XAS) studies indicate that the higher voltage plateaus are related to redox processes on the substituents. In situ x-ray diffraction (XRD) on LiCu{sub 0.5}Mn{sub 1.5}O{sub 4} shows single phase behavior during the charge and discharge process. Three phases are observed for LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} and two phases are observedmore » in the case of LiNi{sub 0.25}Cu{sub 0.25}Mn{sub 1.5}O{sub 4}. The electrolyte stability is dependent on both the operating voltage and the cathode composition. Even though Ni substituted materials have lower voltages, the electrolyte is more stable in cells with the Cu substituted materials.« less

In-Situ Phase Transition Control in the Supercooled State for Robust Active Glass Fiber.

PubMed

Lv, Shichao; Cao, Maoqing; Li, Chaoyu; Li, Jiang; Qiu, Jianrong; Zhou, Shifeng

2017-06-21

The construction of a dopant-activated photonic composite is of great technological importance for various applications, including smart lighting, optical amplification, laser, and optical detection. The bonding arrangement around the introduced dopants largely determines the properties, yet it remains a daunting challenge to manipulate the local state of the matrix (i.e., phase) inside the transparent composite in a controllable manner. Here we demonstrate that the relaxation of the supercooled state enables in-situ phase transition control in glass. Benefiting from the unique local atom arrangement manner, the strategy offers the possibility for simultaneously tuning the chemical environment of the incorporated dopant and engineering the dopant-host interaction. This allows us to effectively activate the dopant with high efficiency (calculated as ∼100%) and profoundly enhance the dopant-host energy-exchange interaction. Our results highlight that the in-situ phase transition control in glass may provide new opportunities for fabrication of unusual photonic materials with intense broadband emission at ∼1100 nm and development of the robust optical detection unit with high compactness and broadband photon-harvesting capability (from X-ray to ultraviolet light).

Direct Observation Through In Situ Transmission Electron Microscope of Early States of Crystallization in Nanoscale Metallic Glasses

NASA Astrophysics Data System (ADS)

Xie, Y.; Sohn, S.; Schroers, J.; Cha, J. J.

2017-11-01

Crystallization is a complex process that involves multiscale physics such as diffusion of atomic species over multiple length scales, thermodynamic energy considerations, and multiple possible intermediate states. In situ crystallization experiments inside a transmission electron microscope (TEM) using nanostructured metallic glasses (MGs) provide a unique platform to study directly crystallization kinetics and pathways. Here, we study the embryonic state of eutectic growth using Pt-Ni-Cu-P MG nanorods under in situ TEM. We directly observe the nucleation and growth of a Ni-rich polymorphic phase, followed by the nucleation and slower growth of a Cu-rich phase. The suppressed growth kinetics of the Cu-rich phase is attributed to locally changing chemical compositions. In addition, we show that growth can be controlled by incorporation of an entire nucleus instead of individual atoms. Such a nucleus has to align with the crystallographic orientation of a larger grain before it can be incorporated into the crystal. By directly observing the crystallization processes, particularly the early stages of non-polymorphic growth, in situ TEM crystallization studies of MG nanostructures provide a wealth of information, some of which can be applied to typical bulk crystallization.

In situ TEM study of G-phase precipitates under heavy ion irradiation in CF8 cast austenitic stainless steel

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

Chen, Wei-Ying; Li, Meimei; Zhang, Xuan

2015-09-01

Thermally-aged cast austenitic stainless steels (CASS) CF8 was irradiated with 1 MeV Kr ions at 300, 350 and 400°C to 1.88x10^15 ions/cm2 (~3 dpa) at the IVEM-Tandem Facility at the Argonne National Laboratory. Before irradiation, the distribution of G-phase precipitates in the ferrite showed strong spatial variations, and both their size and density were affected by the ferrite-austenite phase boundary and presence of M23C6 carbides. Under 300°C irradiation, in-situ TEM observation showed G-phase precipitates were relatively unchanged in the vicinity of the phase boundary M23C6 carbides, while the density of G-phase precipitates increased with increasing dose within the ferrite matrix.more » Coarsening of G-phase precipitates was observed in the vicinity of phase boundary M23C6 carbides at 350°C and 400°C.« less

In situ TEM study of G-phase precipitates under heavy ion irradiation in CF8 cast austenitic stainless steel

NASA Astrophysics Data System (ADS)

Chen, Wei-Ying; Li, Meimei; Zhang, Xuan; Kirk, Marquis A.; Baldo, Peter M.; Lian, Tiangan

2015-09-01

Thermally-aged cast austenitic stainless steels (CASS) CF8 was irradiated with 1 MeV Kr ions at 300, 350 and 400 °C to 1.88 × 1019 ions/m2 (∼3 dpa) at the IVEM-Tandem Facility at the Argonne National Laboratory. Before irradiation, the distribution of G-phase precipitates in the ferrite showed spatial variations, and both their size and density were affected by the ferrite-austenite phase boundary and presence of M23C6 carbides. Under 300 °C irradiation, in situ TEM observation showed G-phase precipitates were relatively unchanged in the vicinity of the phase boundary M23C6 carbides, while the density of G-phase precipitates increased with increasing dose within the ferrite matrix. Coarsening of G-phase precipitates was observed in the vicinity of phase boundary M23C6 carbides at 350 °C and 400 °C.

Integrating Nuclear Energy to Oilfield Operations – Two Case Studies

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

Eric P. Robertson; Lee O. Nelson; Michael G. McKellar

2011-11-01

Fossil fuel resources that require large energy inputs for extraction, such as the Canadian oil sands and the Green River oil shale resource in the western USA, could benefit from the use of nuclear power instead of power generated by natural gas combustion. This paper discusses the technical and economic aspects of integrating nuclear energy with oil sands operations and the development of oil shale resources. A high temperature gas reactor (HTGR) that produces heat in the form of high pressure steam (no electricity production) was selected as the nuclear power source for both fossil fuel resources. Both cases weremore » based on 50,000 bbl/day output. The oil sands case was a steam-assisted, gravity-drainage (SAGD) operation located in the Canadian oil sands belt. The oil shale development was an in-situ oil shale retorting operation located in western Colorado, USA. The technical feasibility of the integrating nuclear power was assessed. The economic feasibility of each case was evaluated using a discounted cash flow, rate of return analysis. Integrating an HTGR to both the SAGD oil sands operation and the oil shale development was found to be technically feasible for both cases. In the oil sands case, integrating an HTGR eliminated natural gas combustion and associated CO2 emissions, although there were still some emissions associated with imported electrical power. In the in situ oil shale case, integrating an HTGR reduced CO2 emissions by 88% and increased natural gas production by 100%. Economic viabilities of both nuclear integrated cases were poorer than the non-nuclear-integrated cases when CO2 emissions were not taxed. However, taxing the CO2 emissions had a significant effect on the economics of the non-nuclear base cases, bringing them in line with the economics of the nuclear-integrated cases. As we move toward limiting CO2 emissions, integrating non-CO2-emitting energy sources to the development of energy-intense fossil fuel resources is becoming increasingly important. This paper attempts to reduce the barriers that have traditionally separated fossil fuel development and application of nuclear power and to promote serious discussion of ideas about hybrid energy systems.« less

Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

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

Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.

2016-04-01

High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c delta hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the alpha-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 degrees C. The f.c.c delta was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region andmore » region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 degrees C.« less

In-situ monitoring of ? phase transformation in Ti-6Al-6V-2Sn using laser ultrasonics

NASA Astrophysics Data System (ADS)

Hinterlechner, Irina; Barriobero-Vila, Pere; Reitinger, Bernhard; Fromherz, Thomas; Requena, Guillermo; Burgholzer, Peter

2018-04-01

Titanium is of great interest for metal processing industries due to its superior material properties, but it is also quite expensive. Therefore, a detailed knowledge of ? phase transformation and consequential the distribution of ? and ? phase in titanium alloys is crucial for their material properties and as a consequence for further processing steps. Measuring the ultrasonic velocity and attenuation by laser ultrasonics technology (LUS) as a non-destructive and non-contact technique, it is possible to qualitatively monitor in-situ the phase transformation during heating the sample from room temperature up to ?. We validate LUS methodology against high energy X-ray diffraction as well as against conventional metallurgic measurements and get excellent agreement between the results of these methods.

Strength and Structure of Ga1-xInx as Alloys

DTIC Science & Technology

1986-04-01

fixtures were ordered and received. An existing furnace and retort will be used to surround the compression fixture. The sample will be positioned in a B203...oncerns the experimental measurement of the flow stress and hardness as a function of temperature and In content:. High mprare hardns testing is used ...approximately 1/3 of the hardness 4 value9 so the latter indicates expected trends for yield stress. flWI1AL WORK The hardess tester used in this study was

Centralized Control and Decentralized Execution: A Catchphrase in Crisis?

DTIC Science & Technology

2009-03-01

assignment of control of forces at any level other than that which is able to exploit fully their weapons is contrary to accepted military doctrine. The...between ground and air com- manders. “The CFACC is not supporting me!” complained some ground commanders, while Airmen retorted , “The CFACC cannot...of war had a strategic im- 3 pact. If the losses suffered early in the operation had continued much longer, or if the Taliban had been able to

Suitability of a Freeze Dried Product as a Vehicle for Vitamin Fortification of Military Ration Packs: A Preliminary Study

DTIC Science & Technology

2011-01-01

75% Retort pouched meals, Noodles , instant Vitamin E > 50% Chocolate, ration > 30% Cheese, processed, cheddar > 50% Scotch-finger biscuit Vitamin A...chocolate milk and low fat milk, 4 °C/36 days (Head and Hansen, 1979) 63% Fortified instant noodles (Sanyoto et al., 2008) 29 to 41% Fruit juices...acid added to instant Asian noodles . in: Panozzo, J.F. and Black, C.K. (Eds), Cereals 2008 - Proceedings of the 58th Australian Cereal Chemistry

Some Stochastic-Duel Models of Combat.

DTIC Science & Technology

1983-03-01

AD-R127 879 SOME STOCHASTIC- DUEL MODELS OF CONBAT(U) NAVAL - / POSTGRADUATE SCHOOL MONTEREY CA J S CHOE MAR 83 UNCLASSiIED FC1/Ehhh1; F/ 12/ ,iE...SCHOOL Monterey, California DTIC ELECTE :MAY 10 1983 "T !H ES IS SOME STOCHASTIC- DUEL MODELS OF COMBAT by Jum Soo Choe March 1983 Thesis Advisor: J. G...TYPE OF RETORT a PERIOD COVIOCe Master’s Thesis Some Stochastic- Duel Models of Combat March 1983 S. PERFORINGi *no. 44POOi umet 7. AUTHORW.) a

Getty Oil Company Diatomite project

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

Zuber, I.L.

1984-09-01

The feasibility of using Diatomite as a synthetic fuels feedstock is discussed. The asphaltic outcropping near McKittrick, California are evidence of oil bearing deposits. Two different processes have been taken to the pilot plant stage to evaluate the viability of recovering oil from the Diatomite ore. One approach was the retorting process which was developed by Lurgi. The other process is based on a totally different concept of solvent extracting the oil from the ore. The operation and performance of the pilot plants are described.

Parameters Affecting the Characteristics of Oil Shale-Derived Fuels.

DTIC Science & Technology

1981-03-01

rock with essentially no organic matter. The oil shale of the Uinta Basin in Utah and extreme western Colorado is richer than the Wyoming shales, but...could be used in several areas of the Uinta Basin . Once the oil shale is mined, it must be heated to about 900’F to hreak down the kerogen. A variety... Uinta Basin of eastern Utah. The sections presented above d.l not exhaust the supply of retorting tech- niques that are in various stages of

Treatment of concentrated industrial wastewaters originating from oil shale and the like by electrolysis polyurethane foam interaction

DOEpatents

Tiernan, Joan E.

1991-01-01

Highly concentrated and toxic petroleum-based and synthetic fuels wastewaters such as oil shale retort water are treated in a unit treatment process by electrolysis in a reactor containing oleophilic, ionized, open-celled polyurethane foams and subjected to mixing and l BACKGROUND OF THE INVENTION The invention described herein arose in the course of, or under, Contract No. DE-AC03-76SF00098 between the U.S. Department of Energy and the University of California.

Vessel with filter and method of use

DOEpatents

Morrell, Jonathan S.; Ripley, Edward B.; Cecala, David M.

2008-01-29

Chemical processing apparatuses which incorporate a process vessel, such as a crucible or retort, and which include a gas separation or filtration system. Various embodiments incorporate such features as loose filtration material, semi-rigid filtration material, and structured filtration material. The vessel may include material that is a microwave susceptor. Filtration media may be selected so that if it inadvertently mixes with the chemical process or the reaction products of such process, it would not adversely affect the results of the chemical process.

Determination of the solubility of tin indium oxide using in situ and ex x-ray diffraction

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

Gonzalez, G. B.; Mason, T. O.; Okasinski, J. S.

A novel approach to determine the thermodynamic solubility of tin in indium oxide via the exsolution from tin overdoped nano-ITO powders is presented. High-energy, in situ and ex situ synchrotron X-ray diffraction was utilized to study the solubility limit at temperatures ranging from 900 C to 1375 C. The tin exsolution from overdoped nanopowders and the formation of In{sub 4}Sn{sub 3}O{sub 12} were observed in situ during the first 4-48 h of high-temperature treatment. Samples annealed between 900 C and 1175 C were also studied ex situ with heat treatments for up to 2060 h. Structural results obtained from Rietveldmore » analysis include compositional phase analysis, atomic positions, and lattice parameters. The tin solubility in In{sub 2}O{sub 3} was determined using the phase analysis compositions from X-ray diffraction and the elemental compositions obtained from X-ray fluorescence. Experimental complications that can lead to incorrect tin solubility values in the literature are discussed.« less

In situ forming phase-inversion implants for sustained ocular delivery of triamcinolone acetonide.

PubMed

Sheshala, Ravi; Hong, Gan Chew; Yee, Wong Pui; Meka, Venkata Srikanth; Thakur, Raghu Raj Singh

2018-02-26

The objectives of this study were to develop biodegradable poly-lactic-co-glycolic acid (PLGA) based injectable phase inversion in situ forming system for sustained delivery of triamcinolone acetonide (TA) and to conduct physicochemical characterisation including in vitro drug release of the prepared formulations. TA (at 0.5%, 1% and 2.5% w/w loading) was dissolved in N-methyl-2-pyrrolidone (NMP) solvent and then incorporated 30% w/w PLGA (50/50 and 75/25) polymer to prepare homogenous injectable solution. The formulations were evaluated for rheological behaviour using rheometer, syringeability by texture analyser, water uptake and rate of implant formation by optical coherence tomography (OCT) microscope. Phase inversion in situ forming formulations were injected into PBS pH 7.3 to form an implant and release samples were collected and analysed for drug content using a HPLC method. All formulations exhibited good syringeability and rheological properties (viscosity: 0.19-3.06 Pa.s) by showing shear thinning behaviour which enable them to remain as free-flowing solution for ease administration. The results from OCT microscope demonstrated that thickness of the implants were increased with the increase in time and the rate of implant formation indicated the fast phase inversion. The drug release from implants was sustained over a period of 42 days. The research findings demonstrated that PLGA/NMP-based phase inversion in situ forming implants can improve compliance in patient's suffering from ocular diseases by sustaining the drug release for a prolonged period of time and thereby reducing the frequency of ocular injections.

Structural comparison of nickel electrodes and precursor phases

NASA Technical Reports Server (NTRS)

Cornilsen, Bahne C.; Shan, Xiaoyin; Loyselle, Patricia

1989-01-01

A summary of previous Raman spectroscopic results and a discussion of important structural differences in the various phases of active mass and active mass precurors are presented. Raman spectra provide unique signatures for these phases, and allow one to distinguish each phase, even when the compound is amorphous to X-rays (i.e., does not scatter X-rays because of a lack of order and/or small particle size). The structural changes incurred during formation, charge and discharge, cobalt addition, and aging will be discussed and related to electrode properties. Important structural differences include NiO2 layer stacking, nonstoichiometry (especially cation-deficit nonstoichiometry), disorder, dopant content, and water content. The results indicate that optimal nickel active mass is non-close packed and nonstoichiometric. The formation process transforms precursor phases into this structure. Therefore, the precursor disorder, or lack thereof, influences this final active mass structure and the rate of formation. Aging processes induce structural change which is believed to be detrimental. The role of cobalt addition can be appreciated in terms of structures favored or stabilized by the dopant. In recent work, the in situ Raman technique to characterize the critical structural parameters was developed. An in situ method relates structure, electrochemistry, and preparation. In situ Raman spectra of cells during charge and discharge, either during cyclic voltammetry or under constant current conditions were collected. With the structure-preparation knowledge and the in situ Raman tool, it will be possible to define the structure-property-preparation relations in more detail. This instrumentation has application to a variety of electrode systems.

Liquid phase in situ hydrodeoxygenation of biomass-derived phenolic compounds to hydrocarbons over bifunctional catalysts

Treesearch

Junfeng Feng; Chung-yun Hse; Zhongzhi Yang; Kui Wang; Jianchun Jiang; Junming Xu

2017-01-01

The objective of this study was to find an effective method for converting renewable biomass-derived phenolic compounds into hydrocarbons bio-fuel via in situ catalytic hydrodeoxygenation. The in situ hydrodeoxygenation of biomass-derived phenolic compounds was carried out in methanol-water solvent over bifunctional catalysts of Raney Ni and HZSM-5 or H-Beta. In the in...

In Situ Observations of Phase Transitions in Metastable Nickel (Carbide)/Carbon Nanocomposites

PubMed Central

2016-01-01

Nanocomposite thin films comprised of metastable metal carbides in a carbon matrix have a wide variety of applications ranging from hard coatings to magnetics and energy storage and conversion. While their deposition using nonequilibrium techniques is established, the understanding of the dynamic evolution of such metastable nanocomposites under thermal equilibrium conditions at elevated temperatures during processing and during device operation remains limited. Here, we investigate sputter-deposited nanocomposites of metastable nickel carbide (Ni3C) nanocrystals in an amorphous carbon (a-C) matrix during thermal postdeposition processing via complementary in situ X-ray diffractometry, in situ Raman spectroscopy, and in situ X-ray photoelectron spectroscopy. At low annealing temperatures (300 °C) we observe isothermal Ni3C decomposition into face-centered-cubic Ni and amorphous carbon, however, without changes to the initial finely structured nanocomposite morphology. Only for higher temperatures (400–800 °C) Ni-catalyzed isothermal graphitization of the amorphous carbon matrix sets in, which we link to bulk-diffusion-mediated phase separation of the nanocomposite into coarser Ni and graphite grains. Upon natural cooling, only minimal precipitation of additional carbon from the Ni is observed, showing that even for highly carbon saturated systems precipitation upon cooling can be kinetically quenched. Our findings demonstrate that phase transformations of the filler and morphology modifications of the nanocomposite can be decoupled, which is advantageous from a manufacturing perspective. Our in situ study also identifies the high carbon content of the Ni filler crystallites at all stages of processing as the key hallmark feature of such metal–carbon nanocomposites that governs their entire thermal evolution. In a wider context, we also discuss our findings with regard to the much debated potential role of metastable Ni3C as a catalyst phase in graphene and carbon nanotube growth. PMID:27746852

In situ Investigation of Magnetism in Metastable Phases of Levitated Fe83 B17 During Solidification

NASA Astrophysics Data System (ADS)

Quirinale, D. G.; Messina, D.; Rustan, G. E.; Kreyssig, A.; Prozorov, R.; Goldman, A. I.

2017-11-01

In situ measurements of structure, density, and magnetization on samples of Fe83 B17 using an electrostatic levitation furnace allow us to identify and correlate the magnetic and structural transitions in this system during its complex solidification process. In particular, we identify magnetic ordering in the metastable Fe23 B6 /fcc Fe coherently grown structures and primitive tetragonal Fe3 B metastable phase in addition to characterizing the equilibrium Fe2 B phase. Our measurements demonstrate that the incorporation of a tunnel-diode oscillator circuit within an electrostatic levitation furnace enables investigations of the physical properties of high-temperature metastable structures.

In situ neutron diffraction study of micromechanical interactions and phase transformation in Ni-Mn-Ga alloy under uniaxial and hydrostatic stress.

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

Peng, R. L.; Wang, Y. D.; Nie, Z. H.

2008-01-01

This paper deals with the experimental study of stress-induced phase transformation in a polycrystalline Ni-Mn-Ga alloy under uniaxial compression and its powder under hydrostatic compression. In situ neutron diffraction experiments were employed to follow changes in the structure and lattice strains caused by the applied stresses. Large lattice strains that are dependent on the lattice planes or grain orientations were observed in the parent Heusler phase for both the bulk material and the powder sample. The development of such anisotropic strains and the influence of external load conditions are discussed in the paper.

Phase formation and texture of thin nickel germanides on Ge(001) and Ge(111)

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

De Schutter, B., E-mail: deschutter.bob@ugent.be; Detavernier, C.; Van Stiphout, K.

2016-04-07

We studied the solid-phase reaction between a thin Ni film and a single crystal Ge(001) or Ge(111) substrate during a ramp anneal. The phase formation sequence was determined using in situ X-ray diffraction and in situ Rutherford backscattering spectrometry (RBS), while the nature and the texture of the phases were studied using X-ray pole figures and transmission electron microscopy. The phase sequence is characterized by the formation of a single transient phase before NiGe forms as the final and stable phase. X-ray pole figures were used to unambiguously identify the transient phase as the ϵ-phase, a non-stoichiometric Ni-rich germanide withmore » a hexagonal crystal structure that can exist for Ge concentrations between 34% and 48% and which forms with a different epitaxial texture on both substrate orientations. The complementary information gained from both RBS and X-ray pole figure measurements revealed a simultaneous growth of both the ϵ-phase and NiGe over a small temperature window on both substrate orientations.« less

An In Situ Directing Group Strategy for Chiral Anion Phase-Transfer Fluorination of Allylic Alcohols

PubMed Central

2015-01-01

An enantioselective fluorination of allylic alcohols under chiral anion phase-transfer conditions is reported. The in situ generation of a directing group proved crucial for achieving effective enantiocontrol. In the presence of such a directing group, a range of acyclic substrates underwent fluorination to afford highly enantioenriched α-fluoro homoallylic alcohols. Mechanistic studies suggest that this transformation proceeds through a concerted enantiodetermining transition state involving both C–F bond formation and C–H bond cleavage. PMID:25203796

In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material

DOE PAGES

Ren, Fei; Schmidt, Robert; Keum, Jong K.; ...

2016-08-24

Introducing nanostructural second phases has been proved to be an effective approach to reduce the lattice thermal conductivity and thus enhance the figure of merit for many thermoelectric materials. Furthermore studies of the formation and evolution of these second phases are central to understanding temperature dependent material behavior, improving thermal stabilities, as well as designing new materials. We examined powder samples of PbTe-PbS thermoelectric material using in situ neutron diffraction and small angle neutron scattering (SANS) techniques from room temperature to elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size of themore » second phase. Neutron diffraction data showed the as-milled powder was primarily solid solution before heat treatment. During heating, PbS second phase precipitated out of the PbTe matrix around 480 K, while re-dissolution started around 570 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger nanostructure remained unchanged. Our study demonstrated that in situ neutron techniques are effective means to obtain quantitative information to study temperature dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less

Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.

A Two-Phase Pilot Study to Evaluate the Safety and Tolerability of an In Situ Polymerizing Collagen.

PubMed

Inglefield, Christopher; Rone-McCrate, Rebecca; Brooks, Robert; Zhu, Jiaxun; Grant, Sheila; DeVore, Dale P

2017-09-01

Demand for collagen-based fillers has declined primarily because of limited long-term clinical benefit and the introduction of hyaluronic acid compositions. In situ polymerizing collagen is a noncrosslinked solution of porcine collagen containing a collagenase shield that undergoes fibrillogenesis on injected into tissues forming a natural matrix. Conduct a prospective, single-center, dual-phase open-label study in 8 subjects to evaluate the safety, tolerability, and efficacy of the porcine collagen composition. In Phase I, potential hypersensitivity of the collagen composition was evaluated after skin testing in the back (men) or forearms of subjects (women). In Phase II, subjects showing no signs of hypersensitivity received collagen injections into the nasolabial area followed by evaluation at 1, 4, 8, and 12 weeks using the Global Aesthetic Improvement Scale. None of the subjects had signs of hypersensitivity and all continued in Phase II. The treating physician(s) reported no post-treatment adverse events. Improvement of the nasolabial fold was observed by the physicians and confirmed by assessment of high-resolution photographs and Global Aesthetic Improvement Scale scores over the 12-week treatment were maintained. In this pilot clinical study in situ polymerizing collagen was shown to be safe and effective throughout the 3-month study period.

In- Situ Synchrotron Diffraction Studies on Transformation Strain Development in a High-Strength Quenched and Tempered Structural Steel—Part II. Martensitic Transformation

NASA Astrophysics Data System (ADS)

Dutta, R. K.; Huizenga, R. M.; Petrov, R. H.; Amirthalingam, M.; King, A.; Gao, H.; Hermans, M. J. M.; Richardson, I. M.

2014-01-01

In-situ synchrotron diffraction studies on the kinetics of phase transformation and transformation strain development during bainitic transformation were presented in part I of the current article. In the current article, in-situ phase transformation behavior of a high-strength (830 MPa yield stress) quenched and tempered S690QL1 [Fe-0.16C-0.2Si-0.87Mn-0.33Cr-0.21Mo (wt. pct)] structural steel, during continuous cooling and under different mechanical loading conditions to promote martensitic transformation, has been studied. Time-temperature-load resolved 2D synchrotron diffraction patterns were recorded and used to calculate the phase fractions and lattice parameters of the phases during heating and cooling cycles under different loading conditions. In addition to the thermal expansion behavior, the effects of the applied stress on the elastic strains during the martensitic transformation were calculated. The results show that small tensile stresses applied at the transformation temperature do not change the kinetics of the phase transformation. The start temperature for the martensitic transformation increases with the increasing applied tensile stress. The elastic strains are not affected significantly with the increasing tensile stress. The variant selection during martensitic transformation under small applied loads (in the elastic region) is weak.

In vitro evaluation of suspoemulsions for in situ-forming polymeric microspheres and controlled release of progesterone.

PubMed

Turino, Ludmila N; Mariano, Rodolfo N; Mengatto, Luciano N; Luna, Julio A

2015-01-01

One possibility to obtain a higher dose of drug in a lower formulation volume can be by using of saturated quantity of drug in one of the phases of an emulsion. These formulations are called suspoemulsions (S/O/W). When a hydrophobic polymer is added to the organic phase of suspoemulsions, these formulations can be used to entrap the drug inside microspheres after in situ precipitation of the polymer-drug-excipients mix. In this work, performance and stability of progesterone suspensions in triacetin as organic phase of suspoemulsions were evaluated. These formulations were compared with O/W emulsions. Mathematical models were used to study in vitro release profiles. The results confirmed that S/O/W systems could be an attractive alternative to O/W formulations for the entrapment of progesterone inside poly(d,l-lactide-co-glycolide) microspheres. Diffusive-based models fit the in vitro release of progesterone from in situ-formed microspheres. For longer release periods, a time-dependent diffusion coefficient was successfully estimated.

Visualizing the chemistry and structure dynamics in lithium-ion batteries by in-situ neutron diffraction

PubMed Central

Wang, Xun-Li; An, Ke; Cai, Lu; Feng, Zhili; Nagler, Stephen E.; Daniel, Claus; Rhodes, Kevin J.; Stoica, Alexandru D.; Skorpenske, Harley D.; Liang, Chengdu; Zhang, Wei; Kim, Joon; Qi, Yue; Harris, Stephen J.

2012-01-01

We report an in-situ neutron diffraction study of a large format pouch battery cell. The succession of Li-Graphite intercalation phases was fully captured under an 1C charge-discharge condition (i.e., charge to full capacity in 1 hour). However, the lithiation and dilithiation pathways are distinctively different and, unlike in slowing charging experiments with which the Li-Graphite phase diagram was established, no LiC24 phase was found during charge at 1C rate. Approximately 75 mol. % of the graphite converts to LiC6 at full charge, and a lattice dilation as large as 4% was observed during a charge-discharge cycle. Our work demonstrates the potential of in-situ, time and spatially resolved neutron diffraction study of the dynamic chemical and structural changes in “real-world” batteries under realistic cycling conditions, which should provide microscopic insights on degradation and the important role of diffusion kinetics in energy storage materials. PMID:23087812

Flow behaviour and structure of heterogeneous particles-water mixture in horizontal and inclined pipes

NASA Astrophysics Data System (ADS)

Vlasák, Pavel; Chára, Zdeněk; Konfršt, Jiří

2018-06-01

The effect of slurry velocity and mean concentration of heterogeneous particle-water mixture on flow behaviour and structure in the turbulent regime was studied in horizontal and inclined pipe sections of inner diameter D = 100 mm. The stratified flow pattern of heterogeneous particle-water mixture in the inclined pipe sections was revealed. The particles moved mostly near to the pipe invert. Concentration distribution in ascending and descending vertical pipe sections confirmed the effect of fall velocity on particle-carrier liquid slip velocity and increase of in situ concentration in the ascending pipe section. Slip velocity in two-phase flow, which is defined as the velocity difference between the solid and liquid phase, is one of mechanism of particle movement in two-phase flow. Due to the slip velocity, there is difference between transport and in situ concentrations, and the slip velocity can be determined from comparison of the in situ and transport concentration. For heterogeneous particle-water mixture flow the slip velocity depends on the flow structure.

An in situ neutron diffraction study of plastic deformation in a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite

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

Wang, D. M.; Chen, Yan; Mu, Juan

Micro-mechanical behaviors of a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite in the plastic regime were investigated by continuous in situ neutron diffraction during compression. Three stages of the plastic deformation were observed according to the work-hardening rate. Here, the underlying natures of the work hardening, correlating with the lattice/microscopic strain evolution, are revealed for the three stages: (1) the initiation of shear bands, (2) the phase load transferring from the amorphous phase to the B2 phase and (3) the accelerated martensitic transformation and the work hardening of the polycrystalline phases promoted by the rapid propagation of the shearmore » bands.« less

An in situ neutron diffraction study of plastic deformation in a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite

DOE PAGES

Wang, D. M.; Chen, Yan; Mu, Juan; ...

2018-05-21

Micro-mechanical behaviors of a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite in the plastic regime were investigated by continuous in situ neutron diffraction during compression. Three stages of the plastic deformation were observed according to the work-hardening rate. Here, the underlying natures of the work hardening, correlating with the lattice/microscopic strain evolution, are revealed for the three stages: (1) the initiation of shear bands, (2) the phase load transferring from the amorphous phase to the B2 phase and (3) the accelerated martensitic transformation and the work hardening of the polycrystalline phases promoted by the rapid propagation of the shearmore » bands.« less

Comparison of extraction phases for a two-phase culture of a recombinant E. coli producing retinoids.

PubMed

Jang, Hui-Jeong; Ha, Bo-Kyung; Kim, Jin-Woong; Jung, Kyung-Hwa; Ahn, Jiyoon; Yoon, Sang-Hwal; Kim, Seon-Won

2014-03-01

To prevent degradation of intracellular retinoids through in situ extraction from the cells, a two-phase culture system was performed. Several organic solvents, including n-alkanes, mineral oils and cosmetic raw materials, were applied as the extraction phase. Of the n-alkanes, n-decane had the highest retinoid production as 134 mg/l after 72 h. For mineral oil, light and heavy mineral oil gave retinoid productions of 158 and 174 mg/l after 96 h, respectively. Of other materials, isopropyl myristate gave the highest retinoid production of 181 mg/l. These results indicate that many types of oils can be applied for retinoid production, and optimization of the in situ extraction process will lead to further improve of economical production for the industrial purpose.

Sign reversal of transformation entropy change in Co{sub 2}Cr(Ga,Si) shape memory alloys

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

Xu, Xiao, E-mail: xu@material.tohoku.ac.jp; Omori, Toshihiro; Kainuma, Ryosuke

2015-11-02

In situ X-ray diffraction (XRD) measurements and compression tests were performed on Co{sub 2}Cr(Ga,Si) shape memory alloys. The reentrant martensitic transformation behavior was directly observed during the in situ XRD measurements. The high-temperature parent phase and low-temperature reentrant parent phase were found to have a continuous temperature dependence of lattice parameter, therefore suggesting that they are the same phase in nature. Moreover, compression tests were performed on a parent-phase single crystal sample; an evolution from normal to inverse temperature dependence of critical stress for martensitic transformation was directly observed. Based on the Clausius-Clapeyron analysis, a sign reversal of entropy changemore » can be expected on the same alloy.« less

In situ TEM observation of heterogeneous phase transition of a constrained single-crystalline Ag2Te nanowire.

PubMed

In, Juneho; Yoo, Youngdong; Kim, Jin-Gyu; Seo, Kwanyong; Kim, Hyunju; Ihee, Hyotchel; Oh, Sang Ho; Kim, Bongsoo

2010-11-10

Laterally epitaxial single crystalline Ag2Te nanowires (NWs) are synthesized on sapphire substrates by the vapor transport method. We observed the phase transitions of these Ag2Te NWs via in situ transmission electron microscopy (TEM) after covering them with Pt layers. The constrained NW shows phase transition from monoclinic to a body-centered cubic (bcc) structure near the interfaces, which is ascribed to the thermal stress caused by differences in the thermal expansion coefficients. Furthermore, we observed the nucleation and growth of bcc phase penetrating into the face-centered cubic matrix at 200 °C by high-resolution TEM in real time. Our results would provide valuable insight into how compressive stresses imposed by overlayers affect behaviors of nanodevices.

Life cycle assessment to evaluate the environmental impact of biochar implementation in conservation agriculture in Zambia.

PubMed

Sparrevik, Magnus; Field, John L; Martinsen, Vegard; Breedveld, Gijs D; Cornelissen, Gerard

2013-02-05

Biochar amendment to soil is a potential technology for carbon storage and climate change mitigation. It may, in addition, be a valuable soil fertility enhancer for agricultural purposes in sandy and/or weathered soils. A life cycle assessment including ecological, health and resource impacts has been conducted for field sites in Zambia to evaluate the overall impacts of biochar for agricultural use. The life cycle impacts from conservation farming using cultivation growth basins and precision fertilization with and without biochar addition were in the present study compared to conventional agricultural methods. Three different biochar production methods were evaluated: traditional earth-mound kilns, improved retort kilns, and micro top-lit updraft (TLUD) gasifier stoves. The results confirm that the use of biochar in conservation farming is beneficial for climate change mitigation purposes. However, when including health impacts from particle emissions originating from biochar production, conservation farming plus biochar from earth-mound kilns generally results in a larger negative effect over the whole life cycle than conservation farming without biochar addition. The use of cleaner technologies such as retort kilns or TLUDs can overcome this problem, mainly because fewer particles and less volatile organic compounds, methane and carbon monoxide are emitted. These results emphasize the need for a holistic view on biochar use in agricultural systems. Of special importance is the biochar production technique which has to be evaluated from both environmental/climate, health and social perspectives.

Monolithic microfluidic concentrators and mixers

DOEpatents

Frechet, Jean M.; Svec, Frantisek; Yu, Cong; Rohr, Thomas

2005-05-03

Microfluidic devices comprising porous monolithic polymer for concentration, extraction or mixing of fluids. A method for in situ preparation of monolithic polymers by in situ initiated polymerization of polymer precursors within microchannels of a microfluidic device and their use for solid phase extraction (SPE), preconcentration, concentration and mixing.

Demonstration of Combined Zero-Valent Iron and Electrical Resistance Heating for In Situ Trichloroethene Remediation

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

Truex, Michael J.; Macbeth, Tamzen; Vermeul, Vincent R.

The effectiveness of in situ treatment using zero-valent iron to remediate sites with non-aqueous phase or significant sediment-associated contaminant mass can be limited by relatively low rates of mass transfer to bring contaminants in contact with the reactive media. For a field test in a trichloroethene source area, combining moderate-temperature (maximum 50oC) subsurface electrical resistance heating with in situ ZVI treatment was shown to accelerate dechlorination and dissolution rates by a factor of 4 to 6 based on organic daughter products and a factor 8-16 using a chloride concentrations. A mass-discharge-based analysis was used to evaluate reaction, dissolution, and volatilizationmore » at ambient groundwater temperature (~10oC) and as temperature was increased up to about 50oC. Increased reaction and contaminant dissolution were observed with increased temperature, but volatilization was minimal during the test because in situ reactions maintained low aqueous-phase TCE concentrations.« less

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

Moorhouse, Saul J.; Wu, Yue; O’Hare, Dermot, E-mail: dermot.ohare@chem.ox.ac.uk

A newly developed in situ monochromatic high-energy X-ray diffraction setup was used to investigate the synthesis of MOFs using cation-impregnated polymer resin beads as a ion source. The Co–NDC–DMF (NDC=2,6-naphthalenedicarboxylate; DMF=dimethylformamide) system was investigated, a system which is known to produce at least three distinct frameworks. It was found that the resin-assisted synthesis results in the preferential formation of a topology previously impossible to synthesise in bulk, while the comparable nitrate-salt synthesis appeared to form an alternative phases. It was also found that the resin-assisted synthesis is highly diffusion-controlled. - Graphical abstract: In situ monochromatic high-energy X-ray diffraction study ofmore » a MOF synthesis. - Highlights: • Resin-assisted solvothermal MOF synthesis was studied using in situ diffraction. • Full kinetics of reaction can be obtained from in situ data. • Kinetics show that this resin-assisted synthesis is diffusion controlled. • Resin-assisted synthesis enables the production of an alternative bulk phase.« less

Reduction reactions and densification during in situ TEM heating of iron oxide nanochains

NASA Astrophysics Data System (ADS)

Bonifacio, Cecile S.; Das, Gautom; Kennedy, Ian M.; van Benthem, Klaus

2017-12-01

The reduction reactions and densification of nanochains assembled from γ-Fe2O3 nanoparticles were investigated using in situ transmission electron microscopy (TEM). Morphological changes and reduction of the metal oxide nanochains were observed during in situ TEM annealing through simultaneous imaging and quantitative analysis of the near-edge fine structures of Fe L2,3 absorption edges acquired by spatially resolved electron energy loss spectroscopy. A change in the oxidation states during annealing of the iron oxide nanochains was observed with phase transformations due to continuous reduction from Fe2O3 over Fe3O4, FeO to metallic Fe. Phase transitions during the in situ heating experiments were accompanied with morphological changes in the nanochains, specifically rough-to-smooth surface transitions below 500 °C, neck formation between adjacent particles around 500 °C, and subsequent neck growth. At higher temperatures, coalescence of FeO particles was observed, representing densification.

In-situ TOF neutron diffraction studies of cyclic softening in superelasticity of a NiFeGaCo shape memory alloy

DOE PAGES

Yang, Hui; Yu, Dunji; Chen, Yan; ...

2016-10-24

Real-time in-situ neutron diffraction was conducted during uniaxial cycling compression of a Ni 49.3Fe 18Ga 27Co 5.7 shape memory alloy to explore the mechanism on its superelasticity at room temperature, which was manifested by the almost recoverable large strains and the apparent cyclic softening. Based on the Rietveld refinements, the real-time evolution of volume fraction of martensite was in-situ monitored, indicating the incremental amount of residual martensite with increasing load cycles. Real-time changes in intensities and lattice strains of { hkl} reflections for individual phase were obtained through fitting individual peaks, which reveal the quantitative information on phase transformation kineticsmore » as a function of grain orientation and stress/strain partitioning. Moreover, a large compressive residual stress was evidenced in the parent phase, which should be balanced by the residual martensite after the second unloading cycle. As a result, the large compressive residual stress found in the parent austenite phase may account for the cyclic effect on critical stress required for triggering the martensitic transformation in the subsequent loading.« less

A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

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

Vadlamani, Bhaskar S; An, Ke; Jagannathan, M.

2014-01-01

The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell hasmore » also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured.« less

In situ Investigation of Magnetism in Metastable Phases of Levitated Fe 83 B 17 During Solidification

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

Quirinale, D. G.; Messina, D.; Rustan, G. E.

In situ measurements of structure, density, and magnetization on samples of Fe 83 B 17 using an electrostatic levitation furnace allow us to identify and correlate the magnetic and structural transitions in this system during its complex solidification process. In particular, we identify magnetic ordering in the metastable Fe 23 B 6 / fcc Fe coherently grown structures and primitive tetragonal Fe 3 B metastable phase in addition to characterizing the equilibrium Fe 2 B phase. Our measurements demonstrate that the incorporation of a tunnel-diode oscillator circuit within an electrostatic levitation furnace enables investigations of the physical properties of high-temperaturemore » metastable structures.« less

Transitional phase inversion of emulsions monitored by in situ near-infrared spectroscopy.

PubMed

Charin, R M; Nele, M; Tavares, F W

2013-05-21

Water-heptane/toluene model emulsions were prepared to study emulsion transitional phase inversion by in situ near-infrared spectroscopy (NIR). The first emulsion contained a small amount of ionic surfactant (0.27 wt % of sodium dodecyl sulfate) and n-pentanol as a cosurfactant. In this emulsion, the study was guided by an inversion coordinate route based on a phase behavior study previously performed. The morphology changes were induced by rising aqueous phase salinity in a "steady-state" inversion protocol. The second emulsion contained a nonionic surfactant (ethoxylated nonylphenol) at a concentration of 3 wt %. A continuous temperature change induced two distinct transitional phase inversions: one occurred during the heating of the system and another during the cooling. NIR spectroscopy was able to detect phase inversion in these emulsions due to differences between light scattered/absorbed by water in oil (W/O) and oil in water (O/W) morphologies. It was observed that the two model emulsions exhibit different inversion mechanisms closely related to different quantities of the middle phases formed during the three-phase behavior of Winsor type III.

In situ synchrotron XRD analysis of the kinetics of spodumene phase transitions.

PubMed

L Moore, Radhika; Mann, Jason P; Montoya, Alejandro; Haynes, Brian S

2018-04-25

The phase transition by thermal activation of natural α-spodumene was followed by in situ synchrotron XRD in the temperature range 896 to 940 °C. We observed both β- and γ-spodumene as primary products in approximately equal proportions. The rate of the α-spodumene inversion is first order and highly sensitive to temperature (apparent activation energy ∼800 kJ mol-1). The γ-spodumene product is itself metastable, forming β-spodumene, with the total product mass fraction ratio fγ/fβ decreasing as the conversion of α-spodumene continues. We found the relationship between the product yields and the degree of conversion of α-spodumene to be the same at all temperatures in the range studied. A model incorporating first order kinetics of the α- and γ-phase inversions with invariant rate constant ratio describes the results accurately. Theoretical phonon analysis of the three phases indicates that the γ phase contains crystallographic instabilities, whilst the α and β phases do not.

In situ neutron diffraction study of deuterium gas absorption by AB5+y alloys used as negative electrode materials for Ni-MH batteries

NASA Astrophysics Data System (ADS)

Latroche, M.; Joubert, J.-M.; Guégan, A. Percheron; Isnard, O.

2004-07-01

LaNi5-type alloys store reversibly hydrogen and are used as negative electrode materials in Ni-MH batteries. Substitutions on La and Ni crystallographic sites have led to competitive materials with complex formulae Mm(Ni4.3-xMn0.4Al0.3Cox)1+y (Mm: mishmetal). Materials involving an unexpected metastable phase γ show the best cycle lives. This phase occurrence depends on the mishmetal composition, the cobalt rate and the over-stoichiometry. It is observed as a transitory phase only for charge in electrochemical process. To confirm the appearance of this phase during gas loading, in beam D2 gas absorption has been performed on two materials for which the γ phase is expected. Phase amounts and cell volumes have been measured by in situ neutron powder diffraction analysis under controlled gas pressure as a function of the state of charge.

IN SITU APPARENT CONDUCTIVITY MEASUREMENTS AND MICROBIAL POPULATION DISTRIBUTION AT A HYDROCARBON CONTAMINATED SITE

EPA Science Inventory

We investigated the bulk electrical conductivity and microbial population distribution in sediments at a site contaminated with light non-aqueous phase liquid (LNAPL). The bulk conductivity was measured using in situ vertical resistivity probes, while the most probable number met...

COMPARISON OF MERCURY CAPTURE EFFICIENCIES OF THREE DIFFERENT IN SITU GENERATED SORBENTS

EPA Science Inventory

Three different sorbent materials (Ti, Si and Ca based) were compared for their mercury capture efficiencies in an entrained flow reactor. Agglomerated particles with a high specific surface area were generated in situ by injecting gas phase sorbent precursors into a high tempera...

New Findings on the Phase Transitions in Li(sub 1-x)CoO(sub 2) and Li(sub 1-x)NiO(sub 2) Cathode Materials During Cycling: In Situ Synchrotron X-Ray Diffraction Studies

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

Yang, X. Q.; Sun, X.; McBreen, J.

The authors have utilized synchrotron x-ray radiation to perform ''in situ'' x-ray diffraction studies on Li{sub 1-x}CoO{sub 2} and Li{sub 1-x}NiO{sub 2} cathodes. A C/10 charging rate was used for a Li/Li{sub 1-x}CoO{sub 2} cell. For the Li/Li{sub 1-x}NiO{sub 2} cells, C/13 and C/84 rates were applied. The in situ XRD data were collected during the first charge from 3.5 to 5.2 V. For the Li{sub 1-x}CoO{sub 2} cathode, in the composition range of x = 0 to x = 0.5, a new intermediate phase H2a was observed in addition to the two expected hexagonal phases H1 and H2. Inmore » the region very close to x = 0.5, some spectral signatures for the formation of a monoclinic phase M1 were also observed. Further, in the x = 0.8 to x = 1 region, the formation of a CdI{sub 2} type hexagonal phase has been confirmed. However, this new phase is transformed from a CdCl{sub 2} type hexagonal phase, rather than from a monoclinic phase M2 as previously reported in the literature. For the Li{sub 1-x}NiO{sub 2} system, by taking the advantage of the high resolution in 2{theta} angles through the synchrotron based XRD technique, they were able to identify a two-phase coexistence region of hexagonal phase H1 and H2, which has been mistakenly indexed as a single phase region for monoclinic phase M1. Interesting similarities and differences between these two systems are also discussed.« less

In Situ X-ray Diffraction Studies of Li(sub x)Mn(sub 2)O(sub 4) Cathode Materials by Synchrotron X-ray Radiation

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

Yang, X. Q.; Sun, X.; Lee, S. J.

In Situ x-ray diffraction studies on Li{sub x}Mn{sub 2}O{sub 4} spinel cathode materials during charge-discharge cycles were carried out by using a synchrotron as x-ray source. Lithium rich (x = 1.03-1.06) spinel materials obtained from two different sources were studied. Three cubic phases with different lattice constants were observed during charge-discharge cycles in all the samples when a Sufficiently low charge-discharge rate (C/10) was used. There are two regions of two-phase coexistence between these three phases, indicating that both phase transitions are first order. The separation of the Bragg peaks representing these three phases varies from sample to sample andmore » also depends on the charge-discharge rate. These results show that the de-intercalation of lithium in lithium-rich spinel cathode materials proceeds through a series of phase transitions from a lithium-rich phase to a lithium-poor phase and finally to a {lambda}-MnO{sub 2} like cubic phase, rather than through a continuous lattice constant contraction in a single phase.« less

Comparison of the thermal stability of the α, β and γ phases in poly(vinylidene fluoride) based on in situ thermal Fourier transform infrared spectroscopy

NASA Astrophysics Data System (ADS)

Biswas, Anirban; Henkel, Karsten; Schmeißer, Dieter; Mandal, Dipankar

2017-12-01

The electroactive β phase of poly(vinylidene fluoride) (PVDF) is induced due to the aging time of PVDF solutions. The feasibility of the combination of the three crystalline polymorphs (α, β and γ) is demonstrated where their relative proportion within the PVDF film can be tailored by the simple monitoring of the preparation conditions. To identify all these phases, Fourier transform infrared (FT-IR) spectroscopy is carried out and it is spotlighted that the vibrational bands at 510 and 841 cm-1 are not sufficient to state the formation of the β phase. The main aim of this work is devoted to develop a better understanding on the thermal stability of these several phases of PVDF, which has a longstanding ambiguity persisting in this area. It has been found that the in situ thermal FT-IR spectroscopy is one of the best alternatives to understand this important issue. It is ascertained that the β phase is the least thermally stable phase among α, β and γ phases, whereas the γ phase is the most thermally stable phase.

In situ Observation of Phase Transformation in MnAl(C) Magnetic Materials

PubMed Central

Si, Ping-Zhan; Qian, Hui-Dong; Choi, Chul-Jin; Park, Jihoon; Han, Sangho; Ge, Hong-Liang; Shinde, Kiran P.

2017-01-01

The phase transformation in two modes, including both displacive and massive growth of τ-phase from ε-MnAl(C), was observed by in situ transmission electron microscopy. The exact temperature range for different phase transformation modes was determined by magnetic measurements. The displacive growth of ε→τ in Mn54Al46 (or Mn54Al46C2.44) occurs at temperatures below 650 K (or 766 K), above which both modes coexist. One-third or less of the ε-phase can be transformed into τ-phase via displacive mode while the remaining two-thirds or more via massive mode. In bulk τ-phase, most τ-nanocrystals formed via displacive mode are distributed in the matrix of large τ-grains that formed via massive mode. The typical massive growth rate of the τ-phase is 8–60 nm/s, while the displacive growth rate is low. A more complete understanding of the ε→τ phase transformations in the MnAl-based magnets was provided in this work, based on which the annealing process for ε→τ was optimized and thus high purity τ-phase with high saturation magnetization was obtained. PMID:28858231

In Situ Neutron Scattering Study of Nanostructured PbTe-PbS Bulk Thermoelectric Material

NASA Astrophysics Data System (ADS)

Ren, Fei; Schmidt, Robert; Case, Eldon D.; An, Ke

2017-05-01

Nanostructures play an important role in thermoelectric materials. Their thermal stability, such as phase change and evolution at elevated temperatures, is thus of great interest to the thermoelectric community. In this study, in situ neutron diffraction was used to examine the phase evolution of nanostructured bulk PbTe-PbS materials fabricated using hot pressing and pulsed electrical current sintering (PECS). The PbS second phase was observed in all samples in the as-pressed condition. The temperature dependent lattice parameter and phase composition data show an initial formation of PbS precipitates followed by a redissolution during heating. The redissolution process started around 570-600 K, and completed at approximately 780 K. During cooling, the PECS sample followed a reversible curve while the heating/cooling behavior of the hot pressed sample was irreversible.

The irreversible formation of palladium carbide during hydrogenation of 1-pentyne over silica-supported palladium nanoparticles: in situ Pd K and L3 edge XAS.

PubMed

Tew, Min Wei; Nachtegaal, Maarten; Janousch, Markus; Huthwelker, Thomas; van Bokhoven, Jeroen A

2012-04-28

The catalytically active phase of silica-supported palladium catalysts in the selective and non-selective hydrogenation of 1-pentyne was determined using in situ X-ray absorption spectroscopy at the Pd K and L(3) edges. Upon exposure to alkyne, a palladium carbide-like phase rapidly forms, which prevents hydrogen to diffuse into the bulk of the nano-sized particles. Both selective and non-selective hydrogenation occur over carbided particles. The palladium carbide-like phase is stable under reaction conditions and only partially decomposes under high hydrogen partial pressure. Non-selective hydrogenation to pentane is not indicative of hydride formation. The palladium carbide phase was detected in the EXAFS analysis and the K edge XANES showed representative features. This journal is © the Owner Societies 2012

In situ study of LaY2Ni9 compound as Ni MH negative-electrode material

NASA Astrophysics Data System (ADS)

Latroche, M.; Isnard, O.

2008-03-01

The behavior of a Ni-MH (metal hydride) negative composite electrode made of LaY2Ni9 active material has been studied dynamically using in situ neutron diffraction during a complete charge-discharge electrochemical cycle. From the analysis of the collected diffraction patterns, the phase identity, phase amount variations and cell volume evolutions have been determined as a function of the electrochemical state of (dis)charge. The active material shows a typical two-phase behavior with equilibrium between a hydrogen-poor α phase and a hydrogen-rich β one. The lower electrochemical reversible capacity as compared to solid-gas properties has been interpreted in terms of hydrogen gas evolving during charge and kinetic limitation due to slow β to α transformation during discharge, which hinders high discharge rates.

In situ optical microscopy of the martensitic phase transformation of lithium

NASA Astrophysics Data System (ADS)

Krystian, M.; Pichl, W.

2000-12-01

The phase transformation of lithium was investigated by in situ optical microscopy in a helium cryostat. The martensite microstructure is composed of irregular segments which grow in rapid bursts from many nuclei to a final size of 10 to 20 μm and then are immobilized. A major part of the segments is arranged in groups of parallel lamellas. A theoretical consideration of lattice compatibility predicts the existence of an almost perfectly coherent habit-plane interface between bcc and 9R in lithium. Therefore, the irregular microstructure is interpreted by the presence of the disordered polytype phase. Comparison with an earlier investigation in comparably impure lithium indicates a strong influence of impurities on the transformation mechanism. The connections between the low-temperature phase diagram, the geometrical compatibility condition, and the martensite microstructure are discussed.

In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material

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

Ren, Fei, E-mail: renfei@temple.edu, E-mail: kean@ornl.gov; Qian, Bosen; Schmidt, Robert

2016-08-22

Introducing nanostructural second phases has proved to be an effective approach to reduce the lattice thermal conductivity and thus enhances the figure of merit for many thermoelectric materials. Studies of the formation and evolution of these second phases are essential to understanding material temperature dependent behaviors, improving thermal stabilities, as well as designing new materials. In this study, powder samples of the PbTe-PbS thermoelectric material were examined using in situ neutron diffraction and small angle neutron scattering (SANS) techniques between room temperature and elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size ofmore » the second phase. Neutron diffraction data showed that the as-milled powder was primarily a solid solution prior to heat treatment. During heating, a PbS second phase precipitated out of the PbTe matrix around 500 K, while re-dissolution started around 600 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated that there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger one remained unchanged. This study demonstrated that in situ neutron techniques are effective means to obtain quantitative information on temperature-dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less

In Vivo Formation of Cubic Phase in Situ after Oral Administration of Cubic Phase Precursor Formulation Provides Long Duration Gastric Retention and Absorption for Poorly Water-Soluble Drugs.

PubMed

Pham, Anna C; Hong, Linda; Montagnat, Oliver; Nowell, Cameron J; Nguyen, Tri-Hung; Boyd, Ben J

2016-01-04

Lipid-based liquid crystalline systems based on the combination of digestible and nondigestible lipids have been proposed as potential sustained release delivery systems for oral delivery of poorly water-soluble drugs. The potential for cubic phase liquid crystal formation to induce dramatically extended gastric retention in vivo has been shown previously to strongly influence the resulting pharmacokinetics of incorporated drug. In vitro studies showing the in situ formation of cubic phase from a disordered precursor comprising a mixture of digestible and nondigestible lipids under enzymatic digestion have also recently been reported. Combining both concepts, here we show the potential for such systems to form in vivo, increasing gastric retention, and providing a sustained release effect for a model poorly water-soluble drug cinnarizine. A mixture of phytantriol and tributyrin at an 85:15 mass ratio, shown previously to form cubic phase under the influence of digestion, induced a similar pharmacokinetic profile to that in the absence of tributyrin, but completely different from tributyrin alone. The gastric retention of the formulation, assessed using micro-X-ray CT imaging, was also consistent with the pharmacokinetic behavior, where phytantriol alone and with 15% tributyrin was greater than that of tributyrin in the absence of phytantriol. Thus, the concept of precursor lipid systems that form cubic phase in situ during digestion in vivo has been demonstrated and opens new opportunities for sustained release of poorly water-soluble drugs.

Aging behavior of an in-situ TiB{sub 2}/Al-Cu-Li-x matrix composite

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

Shen, Yanwei; Hong, Tianran; Geng, Jiwei

Transmission electron microscopy, differential scanning calorimetry and hardness tests have been performed on an in-situ TiB{sub 2}/Al-3.3Cu-1.0Li-0.60Mg-0.40Ag-0.14Zr-0.13Si composite to study its aging behavior at 175 °C. A cubic phase suspected to be the σ (Al{sub 5}Cu{sub 6}Mg{sub 2}) phase or its variant is precipitated at all aging stages studied, and this phase is not typically observed in the Al-Cu-Li alloys. The primary hardening (aging for 3 h) phases consist of δ′ (Al{sub 3}Li), β′ (Al{sub 3}Zr) and the cubic phase. After aging for 18 h, all precipitates including T{sub 1} (Al{sub 2}CuLi), S (Al{sub 2}CuMg), θ′ (Al{sub 2}Cu), δ′, β′more » and the cubic phase have appeared, and the formation of T{sub 1} and S results in a rapid increase in hardness. With prolonging of aging time, the apparent coarsening of T{sub 1} and S results in a decline in hardness. - Highlights: •The aging behavior of an in-situ TiB{sub 2}/Al-Cu-Li-x composite was studied. •A cubic phase suspected to be σ (Al{sub 5}Cu{sub 6}Mg{sub 2}) or its variant was precipitated. •The hardness change was dominated by the evolution of T{sub 1} (Al{sub 2}CuLi) and S (Al{sub 2}CuMg).« less

19. VIEW LOOKING SOUTHWEST TOWARDS THE ANCILLARY BUILDINGS. FROM LEFT ...

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

19. VIEW LOOKING SOUTHWEST TOWARDS THE ANCILLARY BUILDINGS. FROM LEFT TO RIGHT BACKGROUND, RETORT BUILDING, STORAGE, SMELTER BUILDING, GARAGE. THE NORTHWEST CORNER OF THE VANNER ROOM IS IN THE FOREGROUND AND LEFT. A 2000 DODGE GRAND CARAVAN IS IN THE FOREGROUND CENTER. THEIR USE OF THE SHED TO THE REAR OF THE AUTOMOBILE IS UNCERTAIN, ALTHOUGH IT IS CONNECTED TO THE MILL AT THE BASE OF THE WEST SIDE OF THE AMALGAMATING PANS ROOM. - Standard Gold Mill, East of Bodie Creek, Northeast of Bodie, Bodie, Mono County, CA

Inductive System for Reliable Magnesium Level Detection in a Titanium Reduction Reactor

NASA Astrophysics Data System (ADS)

Krauter, Nico; Eckert, Sven; Gundrum, Thomas; Stefani, Frank; Wondrak, Thomas; Frick, Peter; Khalilov, Ruslan; Teimurazov, Andrei

2018-05-01

The determination of the Magnesium level in a Titanium reduction retort by inductive methods is often hampered by the formation of Titanium sponge rings which disturb the propagation of electromagnetic signals between excitation and receiver coils. We present a new method for the reliable identification of the Magnesium level which explicitly takes into account the presence of sponge rings with unknown geometry and conductivity. The inverse problem is solved by a look-up-table method, based on the solution of the inductive forward problems for several tens of thousands parameter combinations.

FIELD-SCALE EVALUATION OF IN SITU COSOLVENT FLUSHING FOR ENCHANCED AQUIFER REMEDIATION

EPA Science Inventory

A comprehensive, field-scale evaluation of in situ cosolvent flushing for enhanced remediation of nonaqueous phase liquid (NAPL)-contaminated aquifers was performed in a hydraulically isolated test cell (about 4.3 m x 3.6 m) constructed at a field site at Hill Air Force Base, Uta...

Mechanism for microwave heating of 1-(4'-cyanophenyl)-4-propylcyclohexane characterized by in situ microwave irradiation NMR spectroscopy.

PubMed

Tasei, Yugo; Yamakami, Takuya; Kawamura, Izuru; Fujito, Teruaki; Ushida, Kiminori; Sato, Motoyasu; Naito, Akira

2015-05-01

Microwave heating is widely used to accelerate organic reactions and enhance the activity of enzymes. However, the detailed molecular mechanism for the effect of microwave on chemical reactions is not yet fully understood. To investigate the effects of microwave heating on organic compounds, we have developed an in situ microwave irradiation NMR spectroscopy. (1)H NMR spectra of 1-(4'-cyanophenyl)-4-propylcyclohexane (PCH3) in the liquid crystalline and isotropic phases were observed under microwave irradiation. When the temperature was regulated at slightly higher than the phase transition temperature (Tc=45 °C) under a gas flow temperature control system, liquid crystalline phase mostly changed to the isotropic phase. Under microwave irradiation and with the gas flow temperature maintained at 20 °C, which is 25 °C below the Tc, the isotropic phase appeared stationary as an approximately 2% fraction in the liquid crystalline phase. The temperature of the liquid crystalline state was estimated to be 38 °C according to the line width, which is at least 7 °C lower than the Tc. The temperature of this isotropic phase should be higher than 45 °C, which is considered to be a non-equilibrium local heating state induced by microwave irradiation. Microwaves at a power of 195 W were irradiated to the isotropic phase of PCH3 at 50 °C and after 2 min, the temperature reached 220 °C. The temperature of PCH3 under microwave irradiation was estimated by measurement of the chemical shift changes of individual protons in the molecule. These results demonstrate that microwave heating generates very high temperature within a short time using an in situ microwave irradiation NMR spectrometer. Copyright © 2015 Elsevier Inc. All rights reserved.

In Situ X-Ray Studies of Crystallization Kinetics and Ordering in Functional Organic and Hybrid Materials

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

Yang, Bin; Keum, Jong K.; Geohegan, David B.

In-Situ and time-resolved X-ray scattering and diffraction is dedicated to yielding the change of structural information as the materials are processed or grown in a controlled environment. In this chapter, we introduce the use of in situ and time-resolved X-ray techniques to understand molecular packing, crystal orientation, and phase transformation during the synthesis and processing of functional organic semiconductors, organic nanowires, and hybrid perovskite materials.

Antimicrobial effect of chlorhexidine digluconate in dentin: In vitro and in situ study.

PubMed

Borges, Fátima Maria Cavalcante; de Melo, Mary Anne Sampaio; Lima, Juliana Paiva Marques; Zanin, Iriana Carla Junqueria; Rodrigues, Lidiany Karla Azevedo

2012-01-01

The aim of this study was to evaluate a very short-term in vitro and in situ effect of 2% chlorhexidine-digluconate-based (CHX) cavity cleanser on the disinfection of dentin demineralized by cariogenic bacteria. Human dentin slabs were randomly allocated and used in 2 distinct phases, in vitro and in situ, for obtaining demineralized dentin. In vitro, the slabs (n=15) were immersed for 5 days in BHI broth inoculated with Streptococcus mutans CTT 3440. In situ, a double-blind design was conducted in one phase of 14 days, during which 20 volunteers wore palatal devices containing two human dental dentin slabs. On 5(th) day in vitro and 14(th) day in situ, the slabs were allocated to the two groups: Control group (5 μl of 0.9% NaCl solution) and CHX group (5 μl of 2% chlorhexidine digluconate solution, Cavity Cleanser™ BISCO, Schaumburg, IL, EUA), for 5 minutes. The microbiological analyses were performed immediately before and after the treatments. The log reductions means found for CHX treatment on tested micro organisms were higher when compared to Control group either in vitro or in situ conditions. Our results showed that CHX was effective in reducing the cultivable microbiota in contaminated dentin. Furthermore, although the use of chlorhexidine-digluconate-based cavity disinfectant did not completely eliminate the viable microorganisms, it served as a suitable agent to disinfect tooth preparations.

Si{sub 3}N{sub 4} layers for the in-situ passivation of GaN-based HEMT structures

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

Yunin, P. A., E-mail: yunin@ipmras.ru; Drozdov, Yu. N.; Drozdov, M. N.

2015-11-15

A method for the in situ passivation of GaN-based structures with silicon nitride in the growth chamber of a metal organic vapor phase epitaxy (MOVPE) reactor is described. The structural and electrical properties of the obtained layers are investigated. The in situ and ex situ passivation of transistor structures with silicon nitride in an electron-beam-evaporation device are compared. It is shown that ex situ passivation changes neither the initial carrier concentration nor the mobility. In situ passivation makes it possible to protect the structure surface against uncontrollable degradation upon the finishing of growth and extraction to atmosphere. In the inmore » situ passivated structure, the carrier concentration increases and the mobility decreases. This effect should be taken into account when manufacturing passivated GaN-based transistor structures.« less

In situ growth of sol-gel-derived nano-VO2 film and its phase transition characteristics

NASA Astrophysics Data System (ADS)

Shi, Qiwu; Huang, Wanxia; Lu, Tiecheng; Yue, Fang; Xiao, Yang; Hu, Yanyan

2014-10-01

We reported the growth of VO2 film deposited by an inorganic sol-gel method, followed by post-annealing. An in situ evolution of the grain size in the films with different annealing temperatures (300, 500, and 700 °C for 90 min), annealing times (500 °C for 20, 40, 60, and 90 min), and film thicknesses (30, 150 and 320 nm) was observed. The results indicated that the grain size distribution in the sol-gel-derived VO2 films was mediated by the density of nucleation center, which was varied in the films with different extents of thermal deformation during the annealing. By increasing the film thickness from 30 to 320 nm, a compact nanostructure with uniform distribution of grain size could be formed. It suggested that the in situ-evolved nanostructure in the thicker VO2 film will lead to lower threshold temperature and enhanced transition intensity in the phase transition. The effect of nanoscale grain size on the lower phase transition temperature in the VO2 film was discussed.

Microstructures and Properties of Plasma Sprayed Ni Based Coatings Reinforced by TiN/C1-xNxTi Generated from In-Situ Solid-Gas Reaction.

PubMed

Wang, Wenquan; Li, Wenmo; Xu, Hongyong

2017-07-11

The strengthening hard phases TiN/C 1- x N x Ti were generated by in-situ solid-gas reaction in Ni-based composite coatings prepared using a plasma spray welding process to reinforce the wear resistance of the coatings. The microstructures and properties of the coatings were investigated. The results showed that the coatings mainly consisted of phases such as TiN, C 1- x N x Ti, TiC, etc. A small amount of CrB, M₇C₃, and M 23 C₆ were also detected in the coatings by micro-analysis method. Compared with the originally pure NiCrBSi coatings, the hardness of the NiCrBSi coatings reinforced by in-situ solid-gas reaction was 900 HV 0.5 , increased by more than 35%. Consequently, the wear resistance of the reinforced coatings was greatly improved due to the finely and uniformly dispersed hard phases mentioned above. The weight losses after wear test for the two kinds of coatings were 15 mg and 8 mg, respectively.

Phase transformations induced by spherical indentation in ion-implanted amorphous silicon

NASA Astrophysics Data System (ADS)

Haberl, B.; Bradby, J. E.; Ruffell, S.; Williams, J. S.; Munroe, P.

2006-07-01

The deformation behavior of ion-implanted (unrelaxed) and annealed ion-implanted (relaxed) amorphous silicon (a-Si) under spherical indentation at room temperature has been investigated. It has been found that the mode of deformation depends critically on both the preparation of the amorphous film and the scale of the mechanical deformation. Ex situ measurements, such as Raman microspectroscopy and cross-sectional transmission electron microscopy, as well as in situ electrical measurements reveal the occurrence of phase transformations in all relaxed a-Si films. The preferred deformation mode of unrelaxed a-Si is plastic flow, only under certain high load conditions can this state of a-Si be forced to transform. In situ electrical measurements have revealed more detail of the transformation process during both loading and unloading. We have used ELASTICA simulations to obtain estimates of the depth of the metallic phase as a function of load, and good agreement is found with the experiment. On unloading, a clear change in electrical conductivity is observed to correlate with a "pop-out" event on load versus penetration curves.

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

Ulvestad, A.; Welland, M. J.; Cha, W.

Crystallographic imperfections can significantly alter material properties and responses to external stimuli, including solute induced phase transformations and crystal growth and dissolution . Despite recent progress in imaging defects using both electron and x-ray techniques, in situ three-dimensional imaging studies of defect dynamics, necessary to understand and engineer nanoscale processes, remains challenging. Here, we report in situ three-dimensional imaging of defect dynamics during the hydriding phase transformation of individual palladium nanocrystals by Bragg Coherent Diffractive Imaging (BCDI) . During constant pressure experiments, we observed that the phase transformation begins after the nucleation of dislocations in large (300 nm) particles. Themore » 3D dislocation network shows that dislocations are close to the phase boundary. The 3D phase morphology resolved by BCDI suggests that the hydrogen-rich phase is more similar to a spherical cap on the hydrogen-poor phase than the core-shell model commonly assumed. We substantiate this conclusion using 3D phase field modeling and demonstrate how phase morphology affects the critical size for dislocation nucleation. We determine the size dependence of the transformation pressure for large (150-300 nm) palladium nanocrystals using variable pressure experiments. Our results reveal a pathway for solute induced structural phase transformations in nanocrystals and demonstrate BCDI as a novel method for understanding dislocation dynamics in phase transforming systems at the nanoscale.« less

Elucidation of structure and nature of the PdO-Pd transformation using in situ PDF and XAS techniques.

PubMed

Keating, Jonathan; Sankar, Gopinathan; Hyde, Timothy I; Kohara, Shinji; Ohara, Koji

2013-06-14

The PdO-Pd phase transformation in a 4 wt% Pd/Al2O3 catalyst has been investigated using in situ X-ray absorption spectroscopy (XAS) and in situ X-ray total scattering (also known as high-energy X-ray diffraction) techniques. Both the partial and total pair distribution functions (PDF) from these respective techniques have been analysed in depth. New information from PDF analysis of total scattering data has been garnered using the differential PDF (d-PDF) approach where only correlations orginating from PdO and metallic Pd are extracted. This method circumvents problems encountered in characerising the catalytically active components due to the diffuse scattering from the disordered γ-Al2O3 support phase. Quantitative analysis of the palladium components within the catalyst allowed for the phase composition to be established at various temperatures. Above 850 °C it was found that PdO had converted to metallic Pd, however, the extent of reduction was of the order ca. 70% Pd metal and 30% PdO. Complementary in situ XANES and EXAFS were performed, with heating to high temperature and subsequent cooling in air, and the results of the analyses support the observations, that residual PdO is detected at elevated temperatures. Hysteresis in the transformation upon cooling is confirmed from XAS studies where reoxidation occurs below 680 °C.

Operando chemistry of catalyst surfaces during catalysis.

PubMed

Dou, Jian; Sun, Zaicheng; Opalade, Adedamola A; Wang, Nan; Fu, Wensheng; Tao, Franklin Feng

2017-04-03

Chemistry of a catalyst surface during catalysis is crucial for a fundamental understanding of mechanism of a catalytic reaction performed on the catalyst in the gas or liquid phase. Due to the pressure- or molecular density-dependent entropy contribution of gas or liquid phase of the reactants and the potential formation of a catalyst surface during catalysis different from that observed in an ex situ condition, the characterization of the surface of a catalyst under reaction conditions and during catalysis can be significant and even necessary for understanding the catalytic mechanism at a molecular level. Electron-based analytical techniques are challenging for studying catalyst nanoparticles in the gas or liquid phase although they are necessary techniques to employ. Instrumentation and further development of these electron-based techniques have now made in situ/operando studies of catalysts possible. New insights into the chemistry and structure of catalyst nanoparticles have been uncovered over the last decades. Herein, the origin of the differences between ex situ and in situ/operando studies of catalysts, and the technical challenges faced as well as the corresponding instrumentation and innovations utilized for characterizing catalysts under reaction conditions and during catalysis, are discussed. The restructuring of catalyst surfaces driven by the pressure of reactant(s) around a catalyst, restructuring in reactant(s) driven by reaction temperature and restructuring during catalysis are also reviewed herein. The remaining challenges and possible solutions are briefly discussed.

Support effects in catalysis studied by in-situ sum frequency generation vibrational spectroscopy and in-situ x-ray spectroscopies

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

Kennedy, Griffin John

Here, kinetic measurements are paired with in-situ spectroscopic characterization tools to investigate colloidally based, supported Pt catalytic model systems in order to elucidate the mechanisms by which metal and support work in tandem to dictate activity and selectivity. The results demonstrate oxide support materials, while inactive in absence of Pt nanoparticles, possess unique active sites for the selective conversion of gas phase molecules when paired with an active metal catalyst.

Creating Drug Solubilization Compartments via Phase Separation in Multicomponent Buccal Patches Prepared by Direct Hot Melt Extrusion-Injection Molding.

PubMed

Alhijjaj, Muqdad; Bouman, Jacob; Wellner, Nikolaus; Belton, Peter; Qi, Sheng

2015-12-07

Creating in situ phase separation in solid dispersion based formulations to allow enhanced functionality of the dosage form, such as improving dissolution of poorly soluble model drug as well as being mucoadhesive, can significantly maximize the in vitro and in vivo performance of the dosage form. This formulation strategy can benefit a wide range of solid dosage forms for oral and alternative routes of delivery. This study using buccal patches as an example created separated phases in situ of the buccal patches by selecting the excipients with different miscibility with each other and the model drug. The quaternary dispersion based buccal patches containing PEG, PEO, Tween 80, and felodipine were prepared by direct hot melt extrusion-injection molding (HME-IM). The partial miscibility between Tween 80 and semicrystalline PEG-PEO led to the phase separation after extrusion. The Tween phases acted as drug solubilization compartments, and the PEG-PEO phase had the primary function of providing mucoadhesion and carrier controlled dissolution. As felodipine was preferably solubilized in the amorphous regions of PEG-PEO, the high crystallinity of PEG-PEO resulted in an overall low drug solubilizing capacity. Tween 80 was added to improve the solubilization capacity of the system as the model drug showed good solubility in Tween. Increasing the drug loading led to the supersaturation of drug in Tween compartments and crystalline drug dispersed in PEG-PEO phases. The spatial distribution of these phase-separated compartments was mapped using X-ray micro-CT, which revealed that the domain size and heterogeneity of the phase separation increased with increasing the drug loading. The outcome of this study provides new insights into the applicability of in situ formed phase separation as a formulation strategy for the delivery of poorly soluble drugs and demonstrated the basic principle of excipient selection for such technology.

CHAMPION INTERNATIONAL SUPERFUND SITE, LIBBY MONTANA FIELD PERFORMANCE EVALUATION BIOREMEDIATION UNIT: IN SITU BIOREMEDIATION OF THE UPPER AQUIFER

EPA Science Inventory

The field performance evaluation of the in-situ bioremediation system at Libby, Montana Superfund Site indicated that treatment appears to have occurred in the water phase under the influence of the treatment injection system. Reduced inorganic compounds may have exerted a deman...

In-Situ Chemical Reduction and Oxidation of VOCs in Groundwater: Groundwater Treatability Studies

NASA Technical Reports Server (NTRS)

Keith, Amy; Glasgow, Jason; McCaleh, Rececca C. (Technical Monitor)

2001-01-01

This paper presents NASA Marshall Space Flight Center's treatability studies for volatile organic compounds in groundwater. In-Situ groundwater treatment technologies include: 1) Chemical Reduction(Ferox); 2) Chemical Oxidation (Fenton Reagents, Permanganate, and Persulfate); and 3) Thermal (Dynamic Underground Stripping, Six-Phase Heating). This paper is presented in viewgraph form.

A MECHANISTIC MODEL FOR MERCURY CAPTURE WITH IN-SITU GENERATED TITANIA PARTICLES: ROLE OF WATER VAPOR

EPA Science Inventory

A mechanistic model to predict the capture of gas phase mercury species using in-situ generated titania nanosize particles activated by UV irradiation is developed. The model is an extension of a recently reported model1 for photochemical reactions that accounts for the rates of...

In situ investigations of phase transformations in Fe-sheathed MgB2 wires

NASA Astrophysics Data System (ADS)

Grivel, J.-C.; Pinholt, R.; Andersen, N. H.; Kovác, P.; Husek, I.; Homeyer, J.

2006-01-01

The phase evolution inside Fe-sheathed wires containing precursor powders consisting of a mixture of Mg and B has been studied in situ by means of x-ray diffraction with hard synchrotron radiation (90 keV). Mg was found to disappear progressively during the heating stage. At 500 °C, the intensity of the Mg diffraction lines is reduced by about 20%. This effect is partly attributable to MgO formation. The MgB2 phase was detected from 575 °C. Fe2B was forming at the interface between the sheath and the ceramic core at sintering temperatures of 780 and 700 °C, but not at 650 °C. The formation rate of this phase is strongly dependent on the heat treatment temperature. Its presence can be readily detected as soon as the average interface reaction thickness exceeds 150-200 nm.

A sediment ecotoxicity assessment platform for in situ measures of chemistry, bioaccumulation and toxicity. Part 2: Integrated application to a shallow estuary.

PubMed

Rosen, Gunther; Chadwick, D Bart; Burton, G Allen; Taulbee, W Keith; Greenberg, Marc S; Lotufo, Guilherme R; Reible, Danny D

2012-03-01

A comprehensive, weight-of-evidence based ecological risk assessment approach integrating laboratory and in situ bioaccumulation and toxicity testing, passive sampler devices, hydrological characterization tools, continuous water quality sensing, and multi-phase chemical analyses was evaluated. The test site used to demonstrate the approach was a shallow estuarine wetland where groundwater seepage and elevated organic and inorganic contaminants were of potential concern. Although groundwater was discharging into the surficial sediments, little to no chemical contamination was associated with the infiltrating groundwater. Results from bulk chemistry analysis, toxicity testing, and bioaccumulation, however, suggested possible PAH toxicity at one station, which might have been enhanced by UV photoactivation, explaining the differences between in situ and laboratory amphipod survival. Concurrently deployed PAH bioaccumulation on solid-phase micro-extraction fibers positively correlated (r(2) ≥ 0.977) with in situ PAH bioaccumulation in amphipods, attesting to their utility as biomimetics, and contributing to the overall improved linkage between exposure and effects demonstrated by this approach. Published by Elsevier Ltd.

In Situ Investigation of the Evolution of Lattice Strain and Stresses in Austenite and Martensite During Quenching and Tempering of Steel

NASA Astrophysics Data System (ADS)

Villa, M.; Niessen, F.; Somers, M. A. J.

2018-01-01

Energy dispersive synchrotron X-ray diffraction was applied to investigate in situ the evolution of lattice strains and stresses in austenite and martensite during quenching and tempering of a soft martensitic stainless steel. In one experiment, lattice strains in austenite and martensite were measured in situ in the direction perpendicular to the sample surface during an austenitization, quenching, and tempering cycle. In a second experiment, the sin2 ψ method was applied in situ during the austenite-to-martensite transformation to distinguish between macro- and phase-specific micro-stresses and to follow the evolution of these stresses during transformation. Martensite formation evokes compressive stress in austenite that is balanced by tensile stress in martensite. Tempering to 748 K (475 °C) leads to partial relaxation of these stresses. Additionally, data reveal that (elastic) lattice strain in austenite is not hydrostatic but hkl dependent, which is ascribed to plastic deformation of this phase during martensite formation and is considered responsible for anomalous behavior of the 200 γ reflection.

Part 3. a novel stereocontrolled, in situ, solution- and solid-phase, Aza Michael approach for high-throughput generation of tetrahydroaminoquinoline-derived natural-product-like architectures.

PubMed

Prakesch, Michael; Srivastava, Stuti; Leek, Donald M; Arya, Prabhat

2006-01-01

With the goal of rapidly accessing tetrahydroquinoline-based natural-product-like polycyclic architectures, herein, we report an unprecedented, in situ, stereocontrolled Aza Michael approach in solution and on the solid phase. The mild reaction conditions required to reach the desired target are highly attractive for the use of this method in library generation. To our knowledge, this approach has not been used before, and it opens a novel route leading to a wide variety of tetrahydroquinoline-derived bridged tricyclic derivatives.

In-situ X-ray diffraction studies of the phase transformations and structural states of B2, R and B19′ phases in Ti{sub 49.5}Ni{sub 50.5} alloy

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

Ostapenko, Marina G., E-mail: artifakt@ispms.tsc.ru; National Research Tomsk Polytechnic University, Tomsk, 634050; Meisner, Ludmila L., E-mail: llm@ispms.tsc.ru

2015-10-27

The martensitic transformation, Debye–Waller factor, mean-square atomic displacements and the coefficient of thermal expansion on cooling of the Ti{sub 49.5}Ni{sub 50.5} shape memory alloy were examined using in-situ X-ray diffraction. It was revealed B2→R (T{sub R} ≡ T = 273 ± 10 K) along with B2→B19’ (M{sub s} ≡ T = 273 ± 10 K) transitions occur. It was found that Debye–Waller factor and mean-square displacement of B2 phase undergo significant increase as functions of temperature when phase transition B2→R and B2→B19’ take place. The analysis of the thermal expansion coefficient of the B2 phase indicates that the value of a increasesmore » almost linearly while cooling.« less

Equilibrium p-T Phase Diagram of Boron: Experimental Study and Thermodynamic Analysis

PubMed Central

Solozhenko, Vladimir L.; Kurakevych, Oleksandr O.

2013-01-01

Solid-state phase transformations and melting of high-purity crystalline boron have been in situ and ex situ studied at pressures to 20 GPa in the 1500–2500 K temperature range where diffusion processes become fast and lead to formation of thermodynamically stable phases. The equilibrium phase diagram of boron has been constructed based on thermodynamic analysis of experimental and literature data. The high-temperature part of the diagram contains p-T domains of thermodynamic stability of rhombohedral β-B106, orthorhombic γ-B28, pseudo-cubic (tetragonal) t'-B52, and liquid boron (L). The positions of two triple points have been experimentally estimated, i.e. β–t'–L at ~ 8.0 GPa and ~ 2490 K; and β–γ–t' at ~ 9.6 GPa and ~ 2230 K. Finally, the proposed phase diagram explains all thermodynamic aspects of boron allotropy and significantly improves our understanding of the fifth element. PMID:23912523

In Situ Environmental TEM in Imaging Gas and Liquid Phase Chemical Reactions for Materials Research.

PubMed

Wu, Jianbo; Shan, Hao; Chen, Wenlong; Gu, Xin; Tao, Peng; Song, Chengyi; Shang, Wen; Deng, Tao

2016-11-01

Gas and liquid phase chemical reactions cover a broad range of research areas in materials science and engineering, including the synthesis of nanomaterials and application of nanomaterials, for example, in the areas of sensing, energy storage and conversion, catalysis, and bio-related applications. Environmental transmission electron microscopy (ETEM) provides a unique opportunity for monitoring gas and liquid phase reactions because it enables the observation of those reactions at the ultra-high spatial resolution, which is not achievable through other techniques. Here, the fundamental science and technology developments of gas and liquid phase TEM that facilitate the mechanistic study of the gas and liquid phase chemical reactions are discussed. Combined with other characterization tools integrated in TEM, unprecedented material behaviors and reaction mechanisms are observed through the use of the in situ gas and liquid phase TEM. These observations and also the recent applications in this emerging area are described. The current challenges in the imaging process are also discussed, including the imaging speed, imaging resolution, and data management. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Secondary phases in Al xCoCrFeNi high-entropy alloys: An in-situ TEM heating study and thermodynamic appraisal

DOE PAGES

Rao, J. C.; Diao, H. Y.; Ocelík, V.; ...

2017-03-27

Secondary phases, either introduced by alloying or heat treatment, are commonly present in most high-entropy alloys (HEAs). Understanding the formation of secondary phases at high temperatures, and their effect on mechanical properties, is a critical issue that is undertaken in the present paper, using the Al xCoCrFeNi (x = 0.3, 0.5, and 0.7) as a model alloy. The in-situ transmission-electron-microscopy (TEM) heating observation, an atom-probe-tomography (APT) study for the reference starting materials (Al 0.3 and Al 0.5 alloys), and thermodynamic calculations for all three alloys, are performed to investigate (1) the aluminum effect on the secondary-phase fractions, (2) the annealing-twinningmore » formation in the face-centered-cubic (FCC) matrix, (3) the strengthening effect of the secondary ordered body-centered-cubic (B2) phase, and (4) the nucleation path of the σ secondary phase thoroughly. Finally, the present work will substantially optimize the alloy design of HEAs and facilitate applications of HEAs to a wide temperature range.« less

Secondary phases in Al xCoCrFeNi high-entropy alloys: An in-situ TEM heating study and thermodynamic appraisal

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

Rao, J. C.; Diao, H. Y.; Ocelík, V.

Secondary phases, either introduced by alloying or heat treatment, are commonly present in most high-entropy alloys (HEAs). Understanding the formation of secondary phases at high temperatures, and their effect on mechanical properties, is a critical issue that is undertaken in the present paper, using the Al xCoCrFeNi (x = 0.3, 0.5, and 0.7) as a model alloy. The in-situ transmission-electron-microscopy (TEM) heating observation, an atom-probe-tomography (APT) study for the reference starting materials (Al 0.3 and Al 0.5 alloys), and thermodynamic calculations for all three alloys, are performed to investigate (1) the aluminum effect on the secondary-phase fractions, (2) the annealing-twinningmore » formation in the face-centered-cubic (FCC) matrix, (3) the strengthening effect of the secondary ordered body-centered-cubic (B2) phase, and (4) the nucleation path of the σ secondary phase thoroughly. Finally, the present work will substantially optimize the alloy design of HEAs and facilitate applications of HEAs to a wide temperature range.« less

Reaction rate kinetics for in situ combustion retorting of Michigan Antrim oil shale

USGS Publications Warehouse

Rostam-Abadi, M.; Mickelson, R.W.

1984-01-01

The intrinsic reaction rate kinetics for the pyrolysis of Michigan Antrim oil shale and the oxidation of the carbonaceous residue of this shale have been determined using a thermogravimetric analysis method. The kinetics of the pyrolysis reaction were evaluated from both isothermal and nonisothermal rate data. The reaction was found to be second-order with an activation energy of 252.2 kJ/mole, and with a frequency factor of 9.25 ?? 1015 sec-1. Pyrolysis kinetics were not affected by heating rates between 0.01 to 0.67??K/s. No evidence of any reactions among the oil shale mineral constituents was observed at temperatures below 1173??K. However, it was found that the presence of pyrite in oil shale reduces the primary devolatilization rate of kerogen and increases the amount of residual char in the spent shale. Carbonaceous residues which were prepared by heating the oil shale at a rate of 0.166??K/s to temperatures between 923??K and 1073??K, had the highest reactivities when oxidized at 0.166??K/s in a gas having 21 volume percent oxygen. Oxygen chemisorption was found to be the initial precursor to the oxidation process. The kinetics governing oxygen chemisorption is (Equation Presented) where X is the fractional coverage. The oxidation of the carbonaceous residue was found also to be second-order. The activation energy and the frequency factor determined from isothermal experiments were 147 kJ/mole and 9.18??107 sec-1 respectively, while the values of these parameters obtained from a nonisothermal experiment were 212 kJ/mole and 1.5??1013 sec-1. The variation in the rate constants is attributed to the fact that isothermal and nonisothermal analyses represent two different aspects of the combustion process.

In situ analysis of phase transformation in sol-gel cogelified nanopowder mixture of Al 2O 3 and TiO 2 using synchrotron X-ray radiation diffraction experiments

NASA Astrophysics Data System (ADS)

Jianu, A.; Stanciu, L.; Groza, J. R.; Lathe, Ch.; Burkel, E.

2003-01-01

Aluminium titanate (Al 2TiO 5) has been selected for study due to its high melting point and thermal shock resistance. In situ analysis of phase transformation and of transformation kinetics of sol-gel powder mixture of alumina and titania cogelified samples was performed using high-temperature synchrotron radiation X-ray diffraction experiments. The high reactivity and molecular mixing of sol-gel cogelified precursor powders contributed to the evolution of the reaction. The stability of the TiO 2-tetragonal structure (anatase) increases due to Al 2O 3 presence. The temperature of the aluminium titanate endothermic reaction decreases when heating rate increases. The results obtained by in situ analysis have been used to establish the sintering parameters in order to obtain fully transformed, dense aluminium titanate bulk ceramics.

Synchrotron In-Situ Aging Study and Correlations to the γ' Phase Instabilities in a High-Refractory Content γ-γ' Ni-Base Superalloy

NASA Astrophysics Data System (ADS)

Antonov, Stoichko; Sun, Eugene; Tin, Sammy

2018-06-01

Detailed ex-situ electron microscopy and atom probe tomography (APT) were combined with in-situ synchrotron diffraction to systematically quantify the chemical, morphological, and lattice instabilities that occur during aging of a polycrystalline high-refractory content Ni-base superalloy. The morphological changes and splitting phenomenon associated with the secondary γ' precipitates were related to a combination of discrete chemical composition variations at the secondary γ'/γ interfaces and additional chemical energy arising from γ precipitates that form within the secondary γ' particles. The compositional phase inhomogeneities led to the precipitation of finely dispersed tertiary γ' particles within the γ matrix and secondary γ particles within the secondary γ' precipitates, which, along with surface grooving of the secondary γ' particles, likely due to a spike in the lattice misfit at the particle interfaces, contributed to the splitting of the precipitates during aging.

Lightweight Mg-based composites with thermodynamically stable interfaces by in-situ combustion synthesis

NASA Astrophysics Data System (ADS)

Jo, Ilguk

Lightweight Mg-based composites have been produced by in-situ combustion synthesis of the Al-Ti-C reaction system. The characteristics of the in-situ composites were investigated in terms of phase evolution and interfacial stability using various analysis techniques. The structural analysis results showed that full conversion of the Al-Ti-C reactants into spherical TiC reinforcements with sizes around 1mum was achieved by the combustion reaction. In-situ formed TiC had less oxygen and higher Al contents at the interface than ex-situ formed TiC; these clean interfaces with an Al layer on the reinforcements were shown to yield interfacial stability. For these reasons, the in-situ composites exhibited higher theoretical densities and also good mechanical properties compared with ex-situ produced composites. The interfacial characteristics of molten Mg with the Al-Ti-C reactants and the commercial TiC+Al substrates were evaluated using an infiltration technique under an argon atmosphere. Infiltration length increased with time at temperature, yielding activation energies (Ea) for each system. The value of Ea for the Al-Ti-C system (307.31kJ/mol) is lower than that for the other system (350.84kJ/mol); the high Ea value indicates that the infiltration is not a simple viscosity-controlled phenomenon but involves a chemical reaction. Formation of the Al3Ti phase was observed from the crystal structural analysis of the infiltrated area; thus, existence of reaction promoting the wetting of Mg. The phase evolution, reaction mechanism and kinetics of the Al-Ti-C reaction were studied using DSC and HT-XRD. It was confirmed that, along with the melting of Al, there was formation of Al3Ti by reaction between Al and Ti. A detailed structural analysis indicates that, the reaction mechanism involves melting of Al followed by formation and growth of Al 3Ti, which then contacts the graphite powder and initiates the combustion reaction. The effect of important process parameters, such as the Al content and the reactant sizes, on the microstructure of the resulting in-situ composites is discussed. Feasibility and castability of the composites were investigated by high pressure die casting the composite preforms into automotive parts and durability tests were conducted on the cast parts.

Three-dimensional imaging of dislocation dynamics during the hydriding phase transformation

DOE PAGES

Ulvestad, A.; Welland, M. J.; Cha, W.; ...

2017-01-16

Crystallographic imperfections can significantly alter material properties and responses to external stimuli, including solute induced phase transformations and crystal growth and dissolution . Despite recent progress in imaging defects using both electron and x-ray techniques, in situ three-dimensional imaging studies of defect dynamics, necessary to understand and engineer nanoscale processes, remains challenging. Here, we report in situ three-dimensional imaging of defect dynamics during the hydriding phase transformation of individual palladium nanocrystals by Bragg Coherent Diffractive Imaging (BCDI) . During constant pressure experiments, we observed that the phase transformation begins after the nucleation of dislocations in large (300 nm) particles. Themore » 3D dislocation network shows that dislocations are close to the phase boundary. The 3D phase morphology resolved by BCDI suggests that the hydrogen-rich phase is more similar to a spherical cap on the hydrogen-poor phase than the core-shell model commonly assumed. We substantiate this conclusion using 3D phase field modeling and demonstrate how phase morphology affects the critical size for dislocation nucleation. We determine the size dependence of the transformation pressure for large (150-300 nm) palladium nanocrystals using variable pressure experiments. Our results reveal a pathway for solute induced structural phase transformations in nanocrystals and demonstrate BCDI as a novel method for understanding dislocation dynamics in phase transforming systems at the nanoscale.« less

Determination of methane concentrations in water in equilibrium with sI methane hydrate in the absence of a vapor phase by in situ Raman spectroscopy

USGS Publications Warehouse

Lu, W.; Chou, I.-Ming; Burruss, R.C.

2008-01-01

Most submarine gas hydrates are located within the two-phase equilibrium region of hydrate and interstitial water with pressures (P) ranging from 8 to 60 MPa and temperatures (T) from 275 to 293 K. However, current measurements of solubilities of methane in equilibrium with hydrate in the absence of a vapor phase are limited below 20 MPa and 283.15 K, and the differences among these data are up to 30%. When these data were extrapolated to other P-T conditions, it leads to large and poorly known uncertainties. In this study, in situ Raman spectroscopy was used to measure methane concentrations in pure water in equilibrium with sI (structure one) methane hydrate, in the absence of a vapor phase, at temperatures from 276.6 to 294.6 (??0.3) K and pressures at 10, 20, 30 and 40 (??0.4%) MPa. The relationship among concentration of methane in water in equilibrium with hydrate, in mole fraction [X(CH4)], the temperature in K, and pressure in MPa was derived as: X(CH4) = exp [11.0464 + 0.023267 P - (4886.0 + 8.0158 P)/T]. Both the standard enthalpy and entropy of hydrate dissolution at the studied T-P conditions increase slightly with increasing pressure, ranging from 41.29 to 43.29 kJ/mol and from 0.1272 to 0.1330 kJ/K ?? mol, respectively. When compared with traditional sampling and analytical methods, the advantages of our method include: (1) the use of in situ Raman signals for methane concentration measurements eliminates possible uncertainty caused by sampling and ex situ analysis, (2) it is simple and efficient, and (3) high-pressure data can be obtained safely. ?? 2007 Elsevier Ltd. All rights reserved.

In situ TEM study of electron-beam radiation induced boron diffusion and effects on phase and microstructure evolution in nanostructured CoFeB/SiO2 thin film

NASA Astrophysics Data System (ADS)

Liu, B. H.; Teo, H. W.; Mo, Z. H.; Mai, Z. H.; Lam, J.; Xue, J. M.; Zhao, Y. Z.; Tan, P. K.

2017-01-01

Using in situ transmission electron microscopy (TEM), we studied boron diffusion and segregation in CoFeB/SiO2 nanostructured thin film stacks. We also investigated how these phenomena affected the phase and microstructure of CoFeB thin films under electron beam irradiation at 300 kV. A unique phase transformation was observed in CoFeB thin films under high-dose electron irradiation, from a polycrystalline Co3Fe to a unilateral amorphous phase of Co3Fe and nanocrystalline FexCo23-xB6. The unilateral amorphization of the Co3Fe film showed an electron-dose-rate sensitivity with a threshold dose rate. Detailed in situ TEM studies revealed that the unilateral amorphization of the Co3Fe film arose from boron segregation at the bottom of the Co3Fe thin film induced by radiation-enhanced diffusion of boron atoms that were displaced by electron knock-on effects. The radiation-induced nanocrystallization of FexCo23-xB6 was also found to be dose-rate sensitive with a higher electron beam current leading to earlier nucleation and more rapid grain growth. The nanocrystallization of FexCo23-xB6 occurred preferentially at the CoFeB/SiO2 interface. Kinetic studies by in situ TEM revealed the surface crystallization and diffusion-controlled nucleation and grain growth mechanisms. The radiation-enhanced atomic diffusivity and high-concentration of radiation-induced point defects at the Co3Fe/SiO2 interface enhanced the local short-range ordering of Fe, Co, and B atoms, favoring nucleation and grain growth of FexCo23-xB6 at the interface.

Gas-phase advanced oxidation for effective, efficient in situ control of pollution.

PubMed

Johnson, Matthew S; Nilsson, Elna J K; Svensson, Erik A; Langer, Sarka

2014-01-01

In this article, gas-phase advanced oxidation, a new method for pollution control building on the photo-oxidation and particle formation chemistry occurring in the atmosphere, is introduced and characterized. The process uses ozone and UV-C light to produce in situ radicals to oxidize pollution, generating particles that are removed by a filter; ozone is removed using a MnO2 honeycomb catalyst. This combination of in situ processes removes a wide range of pollutants with a comparatively low specific energy input. Two proof-of-concept devices were built to test and optimize the process. The laboratory prototype was built of standard ventilation duct and could treat up to 850 m(3)/h. A portable continuous-flow prototype built in an aluminum flight case was able to treat 46 m(3)/h. Removal efficiencies of >95% were observed for propane, cyclohexane, benzene, isoprene, aerosol particle mass, and ozone for concentrations in the range of 0.4-6 ppm and exposure times up to 0.5 min. The laboratory prototype generated a OH(•) concentration derived from propane reaction of (2.5 ± 0.3) × 10(10) cm(-3) at a specific energy input of 3 kJ/m(3), and the portable device generated (4.6 ± 0.4) × 10(9) cm(-3) at 10 kJ/m(3). Based on these results, in situ gas-phase advanced oxidation is a viable control strategy for most volatile organic compounds, specifically those with a OH(•) reaction rate higher than ca. 5 × 10(-13) cm(3)/s. Gas-phase advanced oxidation is able to remove compounds that react with OH and to control ozone and total particulate mass. Secondary pollution including formaldehyde and ultrafine particles might be generated, depending on the composition of the primary pollution.

Molecular recognition in gas sensing: Results from acoustic wave and in-situ FTIR measurements

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

Hierlemann, A.; Ricco, A.J.; Bodenhoefer, K.

Surface acoustic wave (SAW) measurements were combined with direct, in-situ molecular spectroscopy to understand the interactions of surface-confined sensing films with gas-phase analytes. This was accomplished by collecting Fourier-transform infrared external-reflectance spectra (FTIR-ERS) on operating SAW devices during dosing of their specifically coated surfaces with key analytes.

High-Rate Charging Induced Intermediate Phases and Structural Changes of Layer-Structured Cathode for Lithium-Ion Batteries

DOE PAGES

Zhou, Yong-Ning; Yue, Ji-Li; Hu, Enyuan; ...

2016-08-08

Using fast time-resolved in situ X-ray diffraction, charge-rate dependent phase transition processes of layer structured cathode material LiNi 1/3Mn 1/3Co 1/3O 2 for lithium-ion batteries are studied. During first charge, intermediate phases emerge at high rates of 10C, 30C, and 60C, but not at low rates of 0.1C and 1C. These intermediate phases can be continuously observed during relaxation after the charging current is switched off. After half-way charging at high rate, sample studied by scanning transmission electron microscopy shows Li-rich and Li-poor phases' coexistence with tetrahedral occupation of Li in Li-poor phase. Also, the high rate induced overpotential ismore » thought to be the driving force for the formation of this intermediate Li-poor phase. The in situ quick X-ray absorption results show that the oxidation of Ni accelerates with increasing charging rate and the Ni 4+ state can be reached at the end of charge with 30C rate. Finally, these results give new insights in the understanding of the layered cathodes during high-rate charging.« less

Sample environment for in situ synchrotron corrosion studies of materials in extreme environments

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

Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Motta, Arthur T.

A new in situ sample environment has been designed and developed to study the interfacial interactions of nuclear cladding alloys with high temperature steam. The sample environment is particularly optimized for synchrotron X-ray diffraction (XRD) studies for in situ structural analysis. The sample environment is highly corrosion resistant and can be readily adapted for steam environments. The in situ sample environment design complies with G2 ASTM standards for studying corrosion in zirconium and its alloys and offers remote temperature and pressure monitoring during the in situ data collection. The use of the in situ sample environment is exemplified by monitoringmore » the oxidation of metallic zirconium during exposure to steam at 350°C. Finally, the in situ sample environment provides a powerful tool for fundamental understanding of corrosion mechanisms by elucidating the substoichiometric oxide phases formed during early stages of corrosion, which can provide a better understanding the oxidation process.« less

Sample environment for in situ synchrotron corrosion studies of materials in extreme environments

DOE PAGES

Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Motta, Arthur T.; ...

2016-10-25

A new in situ sample environment has been designed and developed to study the interfacial interactions of nuclear cladding alloys with high temperature steam. The sample environment is particularly optimized for synchrotron X-ray diffraction (XRD) studies for in situ structural analysis. The sample environment is highly corrosion resistant and can be readily adapted for steam environments. The in situ sample environment design complies with G2 ASTM standards for studying corrosion in zirconium and its alloys and offers remote temperature and pressure monitoring during the in situ data collection. The use of the in situ sample environment is exemplified by monitoringmore » the oxidation of metallic zirconium during exposure to steam at 350°C. Finally, the in situ sample environment provides a powerful tool for fundamental understanding of corrosion mechanisms by elucidating the substoichiometric oxide phases formed during early stages of corrosion, which can provide a better understanding the oxidation process.« less

Marketable transport fuels made from Julia Creek shale oil

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

Not Available

1987-03-01

CSR Limited and the CSIRO Division of Energy Chemistry have been working on the problem of producing refined products from the Julia Creek deposit in Queensland, Australia. Two samples of shale oil, retorted at different temperatures from Julia Creek oil shale, were found to differ markedly in aromaticity. Using conventional hydrotreating technology, high quality jet and diesel fuels could be made from the less aromatic oil. Naphtha suitable for isomerization and reforming to gasoline could be produced from both oils. This paper discusses oil properties, stabilization of topped crudes, second stage hydrotreatment, and naphtha hydrotreating. 1 figure, 4 tables.

Geochemistry of Israeli oil shales: a review

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

Shirav, M.; Ginzburg, D.

1983-01-01

The oil shales of Israel are widely distributed throughout the country and have current reserves of about 3500 million tons located in the following deposits: Zin, Oron, Ef'e, Hartuv, and Nabi-Musa. The geochemistry and chemical analysis of these shales are discussed, along with the calorific value, oil yield, and trace elements. The main components influencing the quality of the oil shales are organic matter, carbonate, clay minerals, and apatite. Compositional variations within the organic matter are responsible for changes in the relative calorific value and retorted oil yield while fluidized bed combustion is affected by the inorganic components. (JMT)

Treatment of concentrated industrial wastewaters originating from oil shale and the like by electrolysis polyurethane foam interaction

DOEpatents

Tiernan, Joan E.

1990-01-01

Highly concentrated and toxic petroleum-based and synthetic fuels wastewaters such as oil shale retort water are treated in a unit treatment process by electrolysis in a reactor containing oleophilic, ionized, open-celled polyurethane foams and subjected to mixing and laminar flow conditions at an average detention time of six hours. Both the polyurethane foams and the foam regenerate solution are re-used. The treatment is a cost-effective process for waste-waters which are not treatable, or are not cost-effectively treatable, by conventional process series.

Aqueous dispersion polymerization: a new paradigm for in situ block copolymer self-assembly in concentrated solution.

PubMed

Sugihara, Shinji; Blanazs, Adam; Armes, Steven P; Ryan, Anthony J; Lewis, Andrew L

2011-10-05

Reversible addition-fragmentation chain transfer polymerization has been utilized to polymerize 2-hydroxypropyl methacrylate (HPMA) using a water-soluble macromolecular chain transfer agent based on poly(2-(methacryloyloxy)ethylphosphorylcholine) (PMPC). A detailed phase diagram has been elucidated for this aqueous dispersion polymerization formulation that reliably predicts the precise block compositions associated with well-defined particle morphologies (i.e., pure phases). Unlike the ad hoc approaches described in the literature, this strategy enables the facile, efficient, and reproducible preparation of diblock copolymer spheres, worms, or vesicles directly in concentrated aqueous solution. Chain extension of the highly hydrated zwitterionic PMPC block with HPMA in water at 70 °C produces a hydrophobic poly(2-hydroxypropyl methacrylate) (PHPMA) block, which drives in situ self-assembly to form well-defined diblock copolymer spheres, worms, or vesicles. The final particle morphology obtained at full monomer conversion is dictated by (i) the target degree of polymerization of the PHPMA block and (ii) the total solids concentration at which the HPMA polymerization is conducted. Moreover, if the targeted diblock copolymer composition corresponds to vesicle phase space at full monomer conversion, the in situ particle morphology evolves from spheres to worms to vesicles during the in situ polymerization of HPMA. In the case of PMPC(25)-PHPMA(400) particles, this systematic approach allows the direct, reproducible, and highly efficient preparation of either block copolymer vesicles at up to 25% solids or well-defined worms at 16-25% solids in aqueous solution.

In Situ alignment system for phase-shifting point-diffraction interferometry

DOEpatents

Goldberg, Kenneth Alan; Naulleau, Patrick P.

2000-01-01

A device and method to facilitate the gross alignment of patterned object- and image-plane masks in optical systems such as the phase-shifting point diffraction interferometer are provided. When an array of similar pinholes or discreet mask fields is used, confusion can occur over the alignment of the focused beams within the field. Adding to the mask pattern a circumscribed or inscribed set of symbols that are identifiable in situ facilitates the unambiguous gross alignment of the object- and/or image-plane masks. Alternatively, a system of markings can be encoded directly into the window shape to accomplish this same task.

In Situ Chemical Characterization of Mineral Phases in Lunar Granulite Meteorite Northwest Africa 5744

NASA Technical Reports Server (NTRS)

Kent, J. J.; Brandon, A. D.; Lapen, T. J.; Peslier, A. H.; Irving, A. J.; Coleff, D. M.

2012-01-01

Northwest Africa (NWA) 5744 meteorite is a granulitic and troctolitic lunar breccia which may represent nearly pristine lunar crust (Fig. 1). NWA 5744 is unusually magnesian compared to other lunar breccias, with bulk [Mg/(Mg+Fe)] 0.79 [1, 2]. Inspection shows impactor content is likely to be very minor, with low Ni content and a lack of metal grains. Some terrestrial contamination is present, evidenced by calcite within cracks. NWA 5744 has notably low concentrations of incompatible trace elements (ITEs) [2]. The goal of this study is to attempt to classify this lunar granulite through analyses of in situ phases.

A one-step in-situ assembly strategy to construct PEG@MOG-100-Fe shape-stabilized composite phase change material with enhanced storage capacity for thermal energy storage

NASA Astrophysics Data System (ADS)

Wang, Junyong; Andriamitantsoa, Radoelizo S.; Atinafu, Dimberu G.; Gao, Hongyi; Dong, Wenjun; Wang, Ge

2018-03-01

A novel in-situ assembly strategy has been developed to synthesis polyethylene glycol (PEG)@iron-benzenetricarboxylate metal-organic gel (MOG-100-Fe) shape-stabilized composite phase change materials by regulating metal-to-ligand ratio. The PEG@MOG-100-Fe was prepared by an ingenious introduction of PEG into the traditional sol-gel prepared MOG-100-Fe. The composite exhibited high heat storage density and thermal stability. The PEG loading content reached up to 92% without any leakage above its melting point. The heat storage density reaches to 152.88

Electrochemical performance and durability of carbon supported Pt catalyst in contact with aqueous and polymeric proton conductors.

PubMed

Andersen, Shuang Ma; Skou, Eivind

2014-10-08

Significant differences in catalyst performance and durability are often observed between the use of a liquid electrolyte (e.g., sulfuric acid), and a solid polymer electrolyte (e.g., Nafion). To understand this phenomenon, we studied the electrochemical behavior of a commercially available carbon supported platinum catalyst in four different electrode structures: catalyst powder (CP), catalyst ionomer electrode (CIE), half membrane electrode assembly (HMEA), and full membrane electrode assembly (FMEA) in both ex situ and in situ experiments under a simulated start/stop cycle. We found that the catalyst performance and stability are very much influenced by the presence of the Nafion ionomers. The proton conducting phase provided by the ionomer and the self-assembled electrode structure render the catalysts a higher utilization and better stability. This is probably due to an enhanced dispersion, an improved proton-catalyst interface, the restriction of catalyst particle aggregation, and the improved stability of the ionomer phase especially after the lamination. Therefore, an innovative electrode HMEA design for ex-situ catalyst characterization is proposed. The electrode structure is identical to the one used in a real fuel cell, where the protons transport takes place solely through solid state proton conducting phase.

Impact of a simplified in situ protocol on enamel loss after erosive challenge

PubMed Central

Buzalaf, Marília Afonso Rabelo; Oliveira, Thais Marchini; Honório, Heitor Marques; Cruvinel, Thiago

2018-01-01

This study investigated the effect of the period of use and location of intraoral appliances on enamel surface loss. This randomized, single blind in situ study was conducted in 2 crossover phases based on the period of use, in which maxillary and mandibular appliances were simultaneously worn. Bovine enamel blocks (n = 120) were randomly divided among the studied groups by surface hardness. In each phase, fifteen volunteers used one maxillary appliance and two mandibular appliances for 5 days. Erosive challenge was performed 4X/day by immersion in 0.01 M HCL for 2 minutes. In the continuous phase, the intraoral appliances were worn for 20 hours. In the intermittent phase the appliances were worn for 8 hours and 30 minutes. Enamel loss was determined profilometrically. The discomfort of use of the appliances were evaluated in a questionnaire. Data were analyzed by two-way ANOVA/Tukey’s test and chi-square test (p<0.05). The maxillary appliance promoted higher enamel loss compared to the mandibular one (p<0.001). Intermittent use of appliances resulted in similar enamel loss to the continuous one (p = 0.686). All volunteers preferred to use the maxillary appliance in an intermittent regimen. The intermittent use of maxillary appliance is a simplified reliable protocol appropriated for in situ erosion studies in enamel. PMID:29734362

NASA, We Have a Challenge and It's Food Packaging

NASA Technical Reports Server (NTRS)

Perchonok, Michele

2014-01-01

Current Packaging: Freeze Dried Foods Packaging ? The thermoformed base is fabricated from Combitherm PAXX230 [a coextrusion of nylon/medium-density polyethylene (MDPE)/nylon/ethylene-vinyl alcohol (EVOH)/nylon/MDPE/linear low-density polyethylene (LLDPE)]. ? The lid is fabricated from Combitherm PAXX115 (a coextrusion of nylon/EVOH/nylon/LF adhesive/HV polyethylene/LLDPE) ? Natural form (Bite size) foods ? The bite-size food package is fabricated from Combitherm PAXX115, a coextrusion of nylon/EVOH/nylon/LF adhesive/HV polyethylene/LLDPE. ? Overwrap ? Packages are wrapped in a white pouch,.003-mm thick, fabricated from a laminate of polyester/polyethylene/aluminum foil/Surlyn®. This overwrap is removed before the food is prepared and heated. Requirements ? High barrier packaging - low oxygen and water vapor transmission rates ? No aluminum layer ? Mass - <145 grams per m2 ? Flexible ? Puncture resistant ? Approved for food use ? Amenable to sterilization ? Able to be heat sealed ? Preferred (not required) ? Transparent ? Retortable, microwavable, high pressure use. Small Business Innovative Research Program - 7 years ? 8 Phase I contracts ? 4 Phase II contracts ? Two workshops to bring together food packaging experts ? Three internal research tasks ? Public Outreach - average of 3 presentations/yr. for 8 years describing NASA's challenges ? Department of Defense Collaboration - Combat Feeding Program No significant improvement in food packaging capabilities after these efforts. It was unlikely that a food packaging solution could be found within the food science community ? There was a need to go outside to other industries such as pharmaceutical or electrical ? Although a positive result was preferred, a negative result would also be useful ? Two Innovation Techniques were used as a comparison ? InnoCentive - Theoretical Challenge to identify new technologies ? Yet2.com - A matchmaker between NASA and commercial packaging manufacturers

FIELD EVALUATION OF SOLVENT EXTRACTION RESIDUAL BIOTREATMENT (SERB)

EPA Science Inventory

Laboratory and pilot-scale studies have demonstrated that cosolvent-enhanced in situ extraction can remove residual and free-phase nonaqueous phase liquid (NAPL), but may leave levels of contaminants in the ground water and subsurface formations in excess of the regulatory requir...

EVALUATION OF TECHNOLOGIES FOR IN SITU CLEANUP OF DNAPL CONTAMINATED SITES

EPA Science Inventory

Ground-water contamination by nonaqueous phase liquids poses one of the greatest remedial challenges In the field of environmental engineering. Denser-than-water nonaqueous phase liquids (DNAPLs) are especially problematic due to their tow water solubility, high density, and capi...

Critical role of the coupling between the octahedral rotation and A -site ionic displacements in PbZr O3 -based antiferroelectric materials investigated by in situ neutron diffraction

NASA Astrophysics Data System (ADS)

Lu, Teng; Studer, Andrew J.; Yu, Dehong; Withers, Ray L.; Feng, Yujun; Chen, Hua; Islam, S. S.; Xu, Zhuo; Liu, Yun

2017-12-01

This in situ neutron-diffraction study on antiferroelectric (AFE) P b0.99(N b0.02Z r0.65S n0.28T i0.05 ) O3 polycrystalline materials describes systematic structural and associated preferred orientation changes as a function of applied electric field and temperature. It is found that the pristine AFE phase can be poled into the metastable ferroelectric (FE) phase at room temperature. At this stage, both AFE and FE phases consist of modes associated with octahedral rotation and A -site ionic displacements. The temperature-induced phase transition indicates that the octahedral rotation and ionic displacements are weakly coupled in the room-temperature FE phase and decoupled in the high-temperature FE phase. However, both temperature and E -field-induced phase transitions between the AFE and high-temperature FE phase demonstrate the critical role of coupling between octahedral rotation and A -site ionic displacements in stabilizing the AFE structure, which provides not only experimental evidence to support previous theoretical calculations, but also an insight into the design and development of AFE materials. Moreover, the associated preferred orientation evolution in both AFE and FE phases is studied during the phase transitions. It is found that the formation of the preferred orientation can be controlled to tune the samples' FE and AFE properties.

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

NASA Astrophysics Data System (ADS)

Lan, Xi; Gao, Jintao; Huang, Zili; Guo, Zhancheng

2018-03-01

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe3O4 particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO2 at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

NASA Astrophysics Data System (ADS)

Lan, Xi; Gao, Jintao; Huang, Zili; Guo, Zhancheng

2018-06-01

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe3O4 particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO2 at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

The behavior of single-crystal silicon to dynamic loading using in-situ X-ray diffraction and phase contrast imaging

NASA Astrophysics Data System (ADS)

Lee, Hae Ja; Xing, Zhou; Galtier, Eric; Arnold, Brice; Granados, Eduardo; Brown, Shaughnessy B.; Tavella, Franz; McBride, Emma; Fry, Alan; Nagler, Bob; Schropp, Andreas; Seiboth, Frank; Samberg, Dirk; Schroer, Christian; Gleason, Arianna E.; Higginbotham, Andrew

Hydrostatic and uniaxial compression studies have revealed that crystalline silicon undergoes phase transitions from a cubic diamond structure to a variety of phases including orthorhombic Imma phase, body-centered tetragonal phase, and a hexagonal primitive phase. The dynamic response of silicon at high pressure, however, is not well understood. Phase contrast imaging has proven to be a powerful tool for probing density changes caused by the shock propagation into a material. In order to characterize the elastic and phase transitions, we image shock waves in Si with high spatial resolution using the LCLS X-ray free electron laser and Matter in Extreme Conditions instrument. In this study, the long pulse optical laser with pseudo-flat top shape creates high pressures up to 60 GPa. We measure the crystal structure by observing X-ray diffraction orthogonal to the shock propagation direction over a range of pressures. We describe the capability of simultaneously performing phase contrast imaging and in situ X-ray diffraction during shock loading and discuss the dynamic response of Si in high-pressure phases Use of the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515. The MEC instrument is supported by.

A Comprehensive Study on the Electronic State of Hydrogen in α-Phase PdH(D)x-Does a Chemical Bond Between Pd and H(D) Exist?

PubMed

Dekura, Shun; Kobayashi, Hirokazu; Ikeda, Ryuichi; Maesato, Mitsuhiko; Yoshino, Haruka; Ohba, Masaaki; Ishimoto, Takayoshi; Kawaguchi, Shogo; Kubota, Yoshiki; Yoshioka, Satoru; Matsumura, Syo; Sugiyama, Takeharu; Kitagawa, Hiroshi

2018-06-12

The palladium(Pd)-hydrogen(H) system is one of the most famous hydrogen storage systems. Although there has been much research on β-phase PdH(D)x, we comprehensively investigated the nature of the interaction between Pd and H(D) in α-phase PdH(D)x (x < 0.03 at 303 K), and revealed the existence of Pd-H(D) chemical bond for the first time, by various in situ experimental techniques and first-principles theoretical calculations. The lattice expansion by H(D) dissolution in the α-phase lattice suggests the existence of interaction between Pd and H(D). The decrease of magnetic susceptibility and the increase of electrical resistivity indicate that the electronic states are changed by the H(D) dissolution in the α phase. In situ solid-state 1H and 2H NMR results and first-principles theoretical calculations revealed that a Pd-H(D) chemical bond exists in the α phase, but the bonding character of the Pd-H(D) chemical bond in the α phase is quite different from that in the β phase; the nature of the Pd-H(D) chemical bond in the α phase is a localized covalent bond whereas that in the β phase is a metallic bond. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of loteprednol etabonate-loaded cationic nanoemulsified in-situ ophthalmic gel for sustained delivery and enhanced ocular bioavailability.

PubMed

Patel, Nirav; Nakrani, Happy; Raval, Mihir; Sheth, Navin

2016-11-01

A novel cationic nanoemulsified in-situ ophthalmic gel of loteprednol etabonate (LE) was developed to improve the permeability and retention time of formulations for overall improvement of drug's ocular bioavability. Capryol 90 (oil phase), tween 80 (surfactant) and transcutol P (cosurfactant) was selected as formulation excipients to construct pseudoternary phase diagrams and nanoemulsion region was recognized from diagrams. Spontaneous emulsification method was used to manufacture LE nanoemulsion and it was optimized using 3 2 factorial design by considering the amount of oil and the ratio of surfactant to cosurfactant (S mix ) as independent variables and evaluated for various physicochemical properties. Optimized NE was dispersed in Poloxamer 407 and 188 solution to form nanoemulsified sols that were predictable to transform into in-situ gels at corneal temperature. Drug pharmacokinetics of sterilized optimized in situ NE gel, NE-ISG2 [0.69% w/w Capryol 90, 0.99%w/w S mix (3:1), 13% Poloxamer 407, 4% w/w Poloxamer 188] and marketed formulation were assessed in rabbit aqueous humor. The in-situ gels were clear, shear thinning in nature and displayed zero-order drug release kinetics. NE-ISG2 showed the minimum ocular irritation potential and significantly (p < 0.01) higher C max and AUC (0-10 h) , delayed T max , extended mean residence time and improved (2.54-fold times) bioavailability compared to marketed formulation.

Multi-Step Lithiation of Tin Sulfide: An Investigation Using In Situ Electron Microscopy

DOE PAGES

Hwang, Sooyeon; Yao, Zhenpeng; Zhang, Lei; ...

2018-04-03

Two-dimensional metal sulfides have been widely explored as promising electrodes for lithium ion batteries since their two-dimensional layered structure allows lithium ions to intercalate between layers. For tin disulfide, the lithiation process proceeds via a sequence of three different types of reactions: intercalation, conversion, and alloying but the full scenario of reaction dynamics remains nebulous. In this paper, we investigate the dynamical process of the multi-step reactions using in situ electron microscopy and discover an intermediate rock-salt phase with the disordering of Li and Sn cations, after the initial 2-dimensional intercalation. The disordered cations occupy all the octahedral sites andmore » block the channels for intercalation, which alter the reaction pathways during further lithiation. Our first principles calculations of the non-equilibrium lithiation of SnS2 corroborate the energetic preference of the disordered rock-salt structure over known layered polymorphs. The in situ observations and calculations suggest a two-phase reaction nature for intercalation, disordering, and following conversion reactions. In addition, in situ de-lithiation observation confirms that the alloying reaction is reversible while the conversion reaction is not, which is consistent to the ex situ analysis. This work reveals the full lithiation characteristic of SnS2 and sheds light on the understanding of complex multistep reactions in two-dimensional materials.« less

Multi-Step Lithiation of Tin Sulfide: An Investigation Using In Situ Electron Microscopy

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

Hwang, Sooyeon; Yao, Zhenpeng; Zhang, Lei

Two-dimensional metal sulfides have been widely explored as promising electrodes for lithium ion batteries since their two-dimensional layered structure allows lithium ions to intercalate between layers. For tin disulfide, the lithiation process proceeds via a sequence of three different types of reactions: intercalation, conversion, and alloying but the full scenario of reaction dynamics remains nebulous. In this paper, we investigate the dynamical process of the multi-step reactions using in situ electron microscopy and discover an intermediate rock-salt phase with the disordering of Li and Sn cations, after the initial 2-dimensional intercalation. The disordered cations occupy all the octahedral sites andmore » block the channels for intercalation, which alter the reaction pathways during further lithiation. Our first principles calculations of the non-equilibrium lithiation of SnS2 corroborate the energetic preference of the disordered rock-salt structure over known layered polymorphs. The in situ observations and calculations suggest a two-phase reaction nature for intercalation, disordering, and following conversion reactions. In addition, in situ de-lithiation observation confirms that the alloying reaction is reversible while the conversion reaction is not, which is consistent to the ex situ analysis. This work reveals the full lithiation characteristic of SnS2 and sheds light on the understanding of complex multistep reactions in two-dimensional materials.« less

Estimated phase transition and melting temperature of APTES self-assembled monolayer using surface-enhanced anti-stokes and stokes Raman scattering

NASA Astrophysics Data System (ADS)

Sun, Yingying; Yanagisawa, Masahiro; Kunimoto, Masahiro; Nakamura, Masatoshi; Homma, Takayuki

2016-02-01

A structure's temperature can be determined from the Raman spectrum using the frequency and the ratio of the intensities of the anti-Stokes and Stokes signals (the Ias/Is ratio). In this study, we apply this approach and an equation relating the temperature, Raman frequency, and Ias/Is ratio to in-situ estimation of the phase change point of a (3-aminopropyl)triethoxysilane self-assembled monolayer (APTES SAM). Ag nanoparticles were deposited on APTES to enhance the Raman signals. A time-resolved measurement mode was used to monitor the variation in the Raman spectra in situ. Moreover, the structural change in APTES SAM (from ordered to disordered structure) under heating was discussed in detail, and the phase change point (around 118 °C) was calculated.

Acousto-optic Imaging System for In-situ Measurement of the High Temperature Distribution in Micron-size Specimens

NASA Astrophysics Data System (ADS)

Machikhin, Alexander S.; Zinin, Pavel V.; Shurygin, Alexander V.

We developed a unique acousto-optic imaging system for in-situ measurement of high temperature distribution on micron-size specimens. The system was designed to measure temperature distribution inside minerals and functional material phases subjected to high pressure and high temperatures in a diamond anvil cell (DAC) heated by a high powered laser.

In situ stress relaxation mechanism of a superelastic NiTi shape memory alloy under hydrogen charging

NASA Astrophysics Data System (ADS)

Elkhal Letaief, Wissem; Hassine, Tarek; Gamaoun, Fehmi

2017-02-01

On account of its good biocompatibility, superelastic Ni-Ti arc wire alloys have been successfully used in orthodontic clinics. Nevertheless, delayed fracture in the oral cavity caused by hydrogen diffusion can be observed. The in situ stress relaxation susceptibility of a Ni-Ti shape memory alloy towards hydrogen embrittlement has been examined with respect to the current densities and imposed deformations. Orthodontic wires have been relaxed at different martensite volume fractions using current densities of 5, 10 and 20 A/m2 at 20 °C. The in situ relaxation stress shows that, for an imposed strain at the middle of the austenite-martensite transformation, the specimen fractures at the martensite-austenite reverse transformation. However, for an imposed strain at the beginning of the austenite-martensite plateau, the stress decreases in a similar way to the full austenite structure. Moreover, the stress plateau has been recorded at the reverse transformation for a short period. For the fully martensite structure, embrittlement occurs at a higher stress value. This behaviour is attributed to the interaction between the in situ austenite phase expansion and the diffusion of hydrogen in the different volume fractions of the martensite phase, produced at an imposed strain.

Abnormal cubic-tetragonal phase transition of barium strontium titanate nanoparticles studied by in situ Raman spectroscopy and transmission electron microscopy heating experiments

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

Zhang, Yin; Chen, Chen; Gao, Ran

2015-11-02

Phase stability of the ferroelectric materials at high temperature is extremely important to their device performance. Ba{sub x}Sr{sub 1−x}TiO{sub 3} (BST) nanoparticles with different Sr contents (x = 1, 0.91, 0.65, 0.4, and 0) are prepared by a facile hydrothermal method. Using Raman spectroscopy and transmission electron microscopy (TEM) analyses under in situ heating conditions (up to 300 °C), the phase transitions of BST nanoparticles between 25 °C and 280 °C are comprehensively investigated. The original Curie temperature of BST nanoparticles decreases abruptly with the increase in Sr content, which is more obvious than in the bulk or film material. Besides, an abnormal phase transitionmore » from cubic to tetragonal structure is observed from BST nanoparticles and the transition temperature rises along with the increase in Sr content. Direct TEM evidences including a slight lattice distortion have been provided. Differently, BaTiO{sub 3} nanoparticles remained in the tetragonal phase during the above temperature ranges.« less

In Situ Observation of Single-Phase Lithium Intercalation in Sub-25-nm Nanoparticles

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

Zhong, Li; Liu, Yang; Han, Wei-Qiang

Although a non-equilibrium single-phase reaction, with the absence of nucleation and growth of a second phase, is believed to be a key factor for high-rate performance of lithium-ion batteries, it is thermodynamically unfavorable and usually proceeds in electrode materials with small particle sizes (tens of nanometers). Unfortunately, the phase evolutions inside such small particles are often shrouded by the macroscopic inhomogeneous reactions of electrodes containing millions of particles, leading to intensive debate over the size-dependent microscopic reaction mechanisms. Here, we provide a generally applicable methodology based on in-situ electron diffraction study on a multi-particle system to track the lithiation pathwaysmore » in individual nanoparticles, and unambiguously reveal that lithiation of anatase TiO 2, previously long believed to be biphasic, converts to a single-phase reaction when the particle size is below ~25 nm. Our results imply the prevalence of such a size-dependent transition in lithiation mechanism among intercalation compounds whose lithium miscibility gaps are associated with a prominent size effect, and therefore provide important guidelines for designing high-power electrodes, especially cathodes.« less

In Situ Observation of Single-Phase Lithium Intercalation in Sub-25-nm Nanoparticles

DOE PAGES

Zhong, Li; Liu, Yang; Han, Wei-Qiang; ...

2017-05-05

Although a non-equilibrium single-phase reaction, with the absence of nucleation and growth of a second phase, is believed to be a key factor for high-rate performance of lithium-ion batteries, it is thermodynamically unfavorable and usually proceeds in electrode materials with small particle sizes (tens of nanometers). Unfortunately, the phase evolutions inside such small particles are often shrouded by the macroscopic inhomogeneous reactions of electrodes containing millions of particles, leading to intensive debate over the size-dependent microscopic reaction mechanisms. Here, we provide a generally applicable methodology based on in-situ electron diffraction study on a multi-particle system to track the lithiation pathwaysmore » in individual nanoparticles, and unambiguously reveal that lithiation of anatase TiO 2, previously long believed to be biphasic, converts to a single-phase reaction when the particle size is below ~25 nm. Our results imply the prevalence of such a size-dependent transition in lithiation mechanism among intercalation compounds whose lithium miscibility gaps are associated with a prominent size effect, and therefore provide important guidelines for designing high-power electrodes, especially cathodes.« less

Structural changes in a commercial lithium-ion battery during electrochemical cycling: An in situ neutron diffraction study

NASA Astrophysics Data System (ADS)

Sharma, Neeraj; Peterson, Vanessa K.; Elcombe, Margaret M.; Avdeev, Maxim; Studer, Andrew J.; Blagojevic, Ned; Yusoff, Rozila; Kamarulzaman, Norlida

The structural response to electrochemical cycling of the components within a commercial Li-ion battery (LiCoO 2 cathode, graphite anode) is shown through in situ neutron diffraction. Lithuim insertion and extraction is observed in both the cathode and anode. In particular, reversible Li incorporation into both layered and spinel-type LiCoO 2 phases that comprise the cathode is shown and each of these components features several phase transitions attributed to Li content and correlated with the state-of-charge of the battery. At the anode, a constant cell voltage correlates with a stable lithiated graphite phase. Transformation to de-lithiated graphite at the discharged state is characterised by a sharp decrease in both structural cell parameters and cell voltage. In the charged state, a two-phase region exists and is composed of the lithiated graphite phase and about 64% LiC 6. It is postulated that trapping Li in the solid|electrolyte interface layer results in minimal structural changes to the lithiated graphite anode across the constant cell voltage regions of the electrochemical cycle.

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

Kupar, J.; Hasek, M.

The Sanitary Landfill Corrective Action Plan proposes a two pronged approach to remediation. The first part of the total remediation strategy is the placement of a RCRA style closure cap to provide source control of contaminants into the groundwater. The second part of the proposed remediation package is a phased approach primarily using an in situ bioremediation system for groundwater clean up of the Constituents of Concern (COCs) that exceed their proposed Alternate Concentration Limits (ACL). The phased in approach of groundwater clean up will involve operation of the in situ bioremediation system, followed by evaluation of the Phase 1more » system and, if necessary, additional phased remediation strategies. This document presents pertinent information on operations, well locations, anticipated capture zones, monitoring strategies, observation wells and other information which will allow a decision on the acceptability of the remedial strategy as an interim corrective action prior to permit application approval. The proposed interim phase of the remediation program will position two horizontal bioremediation wells such that the respective zones of influence will intersect the migration path for the highest concentrations of each plume.« less

Formation of sodium bismuth titanate-barium titanate during solid-state synthesis

DOE PAGES

Hou, Dong; Aksel, Elena; Fancher, Chris M.; ...

2017-01-12

Phase formation of sodium bismuth titanate (Na 0.5Bi 0.5TiO 3 or NBT) and its solid solution with barium titanate (BaTiO 3 or BT) during the calcination process is studied using in situ high-temperature diffraction. The reactant powders were mixed and heated to 1000°C, while X-ray diffraction patterns were recorded continuously. Phase evolutions from starting materials to final perovskite products are observed, and different transient phases are identified. The formation mechanism of NBT and NBT–xBT perovskite structures is discussed, and a reaction sequence is suggested based on the observations. The in situ study leads to a new processing approach, which ismore » the use of nano-TiO 2, and gives insights to the particle size effect for solid-state synthesis products. Lastly, it was found that the use of nano-TiO 2 as reactant powder accelerates the synthesis process, decreases the formation of transient phases, and helps to obtain phase-pure products using a lower thermal budget.« less

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Molecular Analysis of the In Situ Growth Rates of Subsurface Geobacter Species

PubMed Central

Giloteaux, Ludovic; Barlett, Melissa; Chavan, Milind A.; Smith, Jessica A.; Williams, Kenneth H.; Wilkins, Michael; Long, Philip; Lovley, Derek R.

2013-01-01

Molecular tools that can provide an estimate of the in situ growth rate of Geobacter species could improve understanding of dissimilatory metal reduction in a diversity of environments. Whole-genome microarray analyses of a subsurface isolate of Geobacter uraniireducens, grown under a variety of conditions, identified a number of genes that are differentially expressed at different specific growth rates. Expression of two genes encoding ribosomal proteins, rpsC and rplL, was further evaluated with quantitative reverse transcription-PCR (qRT-PCR) in cells with doubling times ranging from 6.56 h to 89.28 h. Transcript abundance of rpsC correlated best (r2 = 0.90) with specific growth rates. Therefore, expression patterns of rpsC were used to estimate specific growth rates of Geobacter species during an in situ uranium bioremediation field experiment in which acetate was added to the groundwater to promote dissimilatory metal reduction. Initially, increased availability of acetate in the groundwater resulted in higher expression of Geobacter rpsC, and the increase in the number of Geobacter cells estimated with fluorescent in situ hybridization compared well with specific growth rates estimated from levels of in situ rpsC expression. However, in later phases, cell number increases were substantially lower than predicted from rpsC transcript abundance. This change coincided with a bloom of protozoa and increased attachment of Geobacter species to solid phases. These results suggest that monitoring rpsC expression may better reflect the actual rate that Geobacter species are metabolizing and growing during in situ uranium bioremediation than changes in cell abundance. PMID:23275510

EVALUATION OF TECHNOLOGIES FOR IN SITU CLEANUP OF DNAPL CONTAMINATED SITES

EPA Science Inventory

Ground water contamination by non-aqueous phase liquids poses one of the greatest remedial challenges in the field of environmental engineering. Denser-than-water non-aqueous phase liquids (DNAPLs) are especially problematic due to their low water solubility, high density, an...

Raising the superconducting Tc of gallium: In situ characterization of the transformation of α -Ga into β -Ga

NASA Astrophysics Data System (ADS)

Campanini, D.; Diao, Z.; Rydh, A.

2018-05-01

Gallium (Ga) displays several metastable phases. Superconductivity is strongly enhanced in the metastable β -Ga with a critical temperature Tc=6.04 (5 ) K , while stable α -Ga has a much lower Tc<1.2 K . Here we use a membrane-based nanocalorimeter to initiate the transition from α -Ga to β -Ga on demand, as well as study the specific heat of the two phases on one and the same sample. The in situ transformation is initiated by bringing the temperature to about 10 K above the melting temperature of α -Ga. After such treatment, the liquid supercools down to 232 K , where β -Ga solidifies. We find that β -Ga is a strong-coupling type-I superconductor with Δ (0 ) /kBTc=2.00 (5 ) and a Sommerfeld coefficient γn=1.53 (4 ) mJ /molK2 , 2.55 times higher than that in the α phase. The results allow a detailed comparison of fundamental thermodynamic properties between the two phases.

α-Phase transformation kinetics of U – 8 wt% Mo established by in situ neutron diffraction

DOE PAGES

Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; ...

2016-05-08

The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

Synthesis of 1 nm Pd Nanoparticles in a Microfluidic Reactor: Insights from in Situ X ray Absorption Fine Structure Spectroscopy and Small-Angle X ray Scattering

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

Karim, Ayman M.; Al Hasan, Naila M.; Ivanov, Sergei A.

2015-06-11

In this paper we show that the temporal separation of nucleation and growth is not a necessary condition for the colloidal synthesis of monodisperse nanoparticles. The synthesis mechanism of Pd nanoparticles was determined by in situ XAFS and SAXS in a microfluidic reactor capable of millisecond up to an hour time resolution. The SAXS results showed two autocatalytic growth phases, a fast growth phase followed by a very slow growth phase. The steady increase in the number of particles throughout the two growth phases indicates the synthesis is limited by slow continuous nucleation. The transition from fast to slow growthmore » was caused by rapid increase in bonding with the capping agent as shown by XAFS. Based on this fundamental understanding of the synthesis mechanism, we show that 1 nm monodisperse Pd nanoparticles can be synthesized at low temperature using a strong binding capping agent such as trioctylphosphine (TOP).« less

Ionizing laser propagation and spectral phase determination

NASA Astrophysics Data System (ADS)

Mittelberger, D. E.; Nakamura, K.; Lehe, R.; Gonsalves, A. J.; Benedetti, C.; Mao, H.-S.; Daniels, J.; Dale, N.; Swanson, K. K.; Esarey, E.; Leemans, W. P.

2017-03-01

Ionization-induced blueshifting is investigated through INF&RNO simulations and experimental studies at the Berkeley Laboratory Laser Accelerator (BELLA) Center. The effects of spectral phase and optical compression are explored. An in-situ method for verifying the spectral phase of an intense laser pulse at focus is presented, based on the effects of optical compression on the morphology of the blueshifted laser spectra.

In-situ crystal structure determination of seifertite SiO 2 at 129 GPa: Studying a minor phase near Earth’s core–mantle boundary

DOE PAGES

Zhang, Li; Popov, Dmitry; Meng, Yue; ...

2016-01-01

Seifertite SiO₂ likely exists as a minor phase near the core–mantle boundary. By simulating the pressure and temperature conditions near the core–mantle boundary, seifertite was synthesized as a minor phase in a coarse-grained, polycrystalline sample coexisting with the (Mg,Fe)SiO₃ post-perovskite (pPv) phase at 129 GPa and 2500 K. Here we report the first in situ single-crystal structure determination and refinement of seifertite at high pressure and after a temperature quench from laser heating. We improved the data coverage of a minor phase from a diamond-anvil cell (DAC) by merging single-crystal data of seifertite from six selected grains that had differentmore » orientations. Observed systematic absences of reflections from the six individual grains allowed only one space group: Pbcn. The refined results of seifertite are in good agreement with the predictions from previous first-principles calculations at high pressure. This approach provides a method for structure determination of a minor phase in a mineral assemblage synthesized under P-T conditions representative of the deep Earth.« less

Phase transformation of molecular beam epitaxy-grown nanometer-thick Gd₂O₃ and Y₂O₃ on GaN.

PubMed

Chang, Wen-Hsin; Wu, Shao-Yun; Lee, Chih-Hsun; Lai, Te-Yang; Lee, Yi-Jun; Chang, Pen; Hsu, Chia-Hung; Huang, Tsung-Shiew; Kwo, J Raynien; Hong, Minghwei

2013-02-01

High quality nanometer-thick Gd₂O₃ and Y₂O₃ (rare-earth oxide, R₂O₃) films have been epitaxially grown on GaN (0001) substrate by molecular beam epitaxy (MBE). The R₂O₃ epi-layers exhibit remarkable thermal stability at 1100 °C, uniformity, and highly structural perfection. Structural investigation was carried out by in situ reflection high energy electron diffraction (RHEED) and ex-situ X-ray diffraction (XRD) with synchrotron radiation. In the initial stage of epitaxial growth, the R₂O₃ layers have a hexagonal phase with the epitaxial relationship of R₂O₃ (0001)(H)<1120>(H)//GaN(0001)(H)<1120>(H). With the increase in R₂O₃ film thickness, the structure of the R₂O₃ films changes from single domain hexagonal phase to monoclinic phase with six different rotational domains, following the R₂O₃ (201)(M)[020](M)//GaN(0001)(H)<1120>(H) orientational relationship. The structural details and fingerprints of hexagonal and monoclinic phase Gd₂O₃ films have also been examined by using electron energy loss spectroscopy (EELS). Approximate 3-4 nm is the critical thickness for the structural phase transition depending on the composing rare earth element.

In-situ crystal structure determination of seifertite SiO 2 at 129 GPa: Studying a minor phase near Earth’s core–mantle boundary

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

Zhang, Li; Popov, Dmitry; Meng, Yue

Seifertite SiO₂ likely exists as a minor phase near the core–mantle boundary. By simulating the pressure and temperature conditions near the core–mantle boundary, seifertite was synthesized as a minor phase in a coarse-grained, polycrystalline sample coexisting with the (Mg,Fe)SiO₃ post-perovskite (pPv) phase at 129 GPa and 2500 K. Here we report the first in situ single-crystal structure determination and refinement of seifertite at high pressure and after a temperature quench from laser heating. We improved the data coverage of a minor phase from a diamond-anvil cell (DAC) by merging single-crystal data of seifertite from six selected grains that had differentmore » orientations. Observed systematic absences of reflections from the six individual grains allowed only one space group: Pbcn. The refined results of seifertite are in good agreement with the predictions from previous first-principles calculations at high pressure. This approach provides a method for structure determination of a minor phase in a mineral assemblage synthesized under P-T conditions representative of the deep Earth.« less

Phase transformation in δ-Pu alloys at low temperature: An in situ microstructural characterization using X-ray diffraction

NASA Astrophysics Data System (ADS)

Ravat, B.; Platteau, C.; Texier, G.; Oudot, B.; Delaunay, F.

2009-09-01

In order to investigate the martensitic transformation, an isothermal hold at -130 °C for 48 h was performed on a highly homogenized PuGa alloy. The modifications of the microstructure were characterized in situ thanks to a specific tool. This device was developed at the CEA-Valduc to analyze the crystalline structure of plutonium alloys as a function of temperature and more especially at low temperature using X-ray diffraction. The analysis of the recorded diffraction patterns highlighted that the martensitic transformation for this alloy is the result of a direct δ → α' + δ phase transformation. Moreover, a significant Bragg's peaks broadening corresponding to the δ-phase was observed. A microstructural analysis was made to characterize anisotropic microstrain resulting from the stress induced by the unit cell volume difference between the δ and α' phases. The amount of α'-phase evolved was analyzed within the framework of the Avrami theory in order to characterize the nucleation process. The results suggested that the growth mechanism corresponded to a general mechanism where the nucleation sites were in the δ-grain edges and the α'-phase had a plate-like morphology.

Quality and shelf life of buffalo meat blocks processed in retort pouches.

PubMed

Devadason, I Prince; Anjaneyulu, A S R; Mendirtta, S K; Murthy, T R K

2014-12-01

The shelf life of buffalo meat blocks processed in 3-ply retort pouches at Fo = 12.13 in a stock sterilizer were evaluated at 15 days interval for physico-chemical, microbiological and sensory attributes for a period of 3 months. The pH of the product was 6.28 at 0 day and a gradual decline was noticed during storage. Texture of the product as indicated by shear force values had decreased slowly. The residual nitrite content had significantly declined from 82.67 ppm at 0 day to 45.00 ppm on 90th day of storage. The TBARS values were 0.24 and 0.67 mg malonaldehyde/kg, respectively at 0 day and 90 days of storage. Tyrosine value had significantly increased from 0.37 mg/100 g at 0 day to 0.58 mg/100 g during storage. Free aminoacid content increased gradually from an initial level of 124.32 to 217.51 at 90(th) day of storage. The SDS-PAGE hydrolysis pattern showed barely discernible 205 KDa protein and presence of subfragments in the molecular range of 63 KDa to 29 KDa protein. The sensory studies indicated that the products were well acceptable up to a period of 90 days. As the storage period increased pH, reidual nitrite, sensory attributes declined significantly and TBARS value, tyrosine value and free aminoacid content significantly increased. Mesophillic aerobes and anerobes were found to be absent. The shelf life study indicated that the products were well acceptable up to a period of 90 days based on the assessment of physico-chemical, microbiological and sensory attributes.

Detection of falciparum malarial forms in naturally infected anophelines in Cameroon using a fluorescent anti-25-kD monoclonal antibody.

PubMed

Robert, V; Le Goff, G; Essong, J; Tchuinkam, T; Faas, B; Verhave, J P

1995-04-01

Anopheles gambiae s.s. and An. funestus were sampled in houses located in a Plasmodium falciparum-holoendemic site in southern Cameroon. The midguts of female mosquitoes in half-gravid or gravid stages of blood digestion were incubated with a fluorescent monoclonal antibody directed against the P. falciparum zygote/ookinete surface protein Pfs25 and examined using a fluorescent light microscope. Malarial forms were detected in 11.6% of the half-gravid mosquitoes and in 0.0% of the gravid ones (P = 0.012). No difference in infections or the occurrence of malarial forms between An. gambiae and An. funestus was observed. Overall, 127 malarial forms were counted and distributed among round forms, retorts, and ookinetes in 77.2%, 9.5%, and 13.4%, respectively. Round forms include macrogametes, activating microgametocytes, and zygotes. The mean number of malarial forms per infected midgut was 2.16 and the maximum number observed was 13. In four anophelines, round forms, retorts, and ookinetes were simultaneously observed. Sporozoite rates were 5.7% for An. gambiae and 3.8% for An. funestus. In the human population, the gametocyte index for P. falciparum was 38% with a mean density of 1.11 gametocytes per microliter of blood. Differences concerning malarial forms in mosquito midguts were observed between houses (range percentage = 4.7--21.3%; mean range of forms per positive anopheline = 1.1--3.1). In each house, relationships existed between infected vectors and the gametocyte reservoir of their inhabitants. The role in transmission of people with very low gametocytemia, approximately one per microliter, as a reservoir of falciparum malaria in highly endemic areas, is emphasized.

Evolution of In-Situ Generated Reinforcement Precipitates in Metal Matrix Composites

NASA Technical Reports Server (NTRS)

Sen, S.; Kar, S. K.; Catalina, A. V.; Stefanescu, D. M.; Dhindaw, B. K.

2004-01-01

Due to certain inherent advantages, in-situ production of Metal Matrix Composites (MMCs) have received considerable attention in the recent past. ln-situ techniques typically involve a chemical reaction that results in precipitation of a ceramic reinforcement phase. The size and spatial distribution of these precipitates ultimately determine the mechanical properties of these MMCs. In this paper we will investigate the validity of using classical growth laws and analytical expressions to describe the interaction between a precipitate and a solid-liquid interface (SLI) to predict the size and spatial evolution of the in-situ generated precipitates. Measurements made on size and distribution of Tic precipitates in a Ni&I matrix will be presented to test the validity of such an approach.

In situ quantification of β-carotene partitioning in oil-in-water emulsions by confocal Raman microscopy.

PubMed

Wan Mohamad, W A Fahmi; Buckow, Roman; Augustin, MaryAnn; McNaughton, Don

2017-10-15

Confocal Raman microscopy (CRM) was able to quantify the β-carotene concentration in oil droplets and determine the partitioning characteristics of β-carotene within the emulsion system in situ. The results were validated by a conventional method involving solvent extraction of β-carotene separately from the total emulsion as well as the aqueous phase separated by centrifugation, and quantification by absorption spectrophotometry. CRM also enabled the localization of β-carotene in an emulsion. From the Raman image, the β-carotene partitioning between the aqueous and oil phases of palm olein-in-water emulsions stabilized by whey protein isolate (WPI) was observed. Increasing the concentration of β-carotene in an emulsion (from 0.1 to 0.3g/kg emulsion) with a fixed gross composition (10% palm olein:2% WPI) decreased the concentration of β-carotene in the oil droplet. CRM is a powerful tool for in situ analyses of components in heterogeneous systems such as emulsions. Copyright © 2017 Elsevier Ltd. All rights reserved.

SolTrack: an automatic video processing software for in situ interface tracking.

PubMed

Griesser, S; Pierer, R; Reid, M; Dippenaar, R

2012-10-01

High-Resolution in situ observation of solidification experiments has become a powerful technique to improve the fundamental understanding of solidification processes of metals and alloys. In the present study, high-temperature laser-scanning confocal microscopy (HTLSCM) was utilized to observe and capture in situ solidification and phase transformations of alloys for subsequent post processing and analysis. Until now, this analysis has been very time consuming as frame-by-frame manual evaluation of propagating interfaces was used to determine the interface velocities. SolTrack has been developed using the commercial software package MATLAB and is designed to automatically detect, locate and track propagating interfaces during solidification and phase transformations as well as to calculate interfacial velocities. Different solidification phenomena have been recorded to demonstrate a wider spectrum of applications of this software. A validation, through comparison with manual evaluation, is included where the accuracy is shown to be very high. © 2012 The Authors Journal of Microscopy © 2012 Royal Microscopical Society.

In situ synthesis and characterization of uranium carbide using high temperature neutron diffraction

NASA Astrophysics Data System (ADS)

Reiche, H. Matthias; Vogel, Sven C.; Tang, Ming

2016-04-01

We investigated the formation of UCx from UO2+x and graphite in situ using neutron diffraction at high temperatures with particular focus on resolving the conflicting reports on the crystal structure of non-quenchable cubic UC2. The agents were UO2 nanopowder, which closely imitates nano grains observed in spent reactor fuels, and graphite powder. In situ neutron diffraction revealed the onset of the UO2 + 2C → UC + CO2 reaction at 1440 °C, with its completion at 1500 °C. Upon further heating, carbon diffuses into the uranium carbide forming C2 groups at the octahedral sites. This resulting high temperature cubic UC2 phase is similar to the NaCl-type structure as proposed by Bowman et al. Our novel experimental data provide insights into the mechanism and kinetics of formation of UC as well as characteristics of the high temperature cubic UC2 phase which agree with proposed rotational rehybridization found from simulations by Wen et al.

In situ observation of stishovite formation in shock-compressed fused silica

NASA Astrophysics Data System (ADS)

Tracy, Sally June; Turneaure, Stefan; Duffy, Thomas

2017-06-01

Silica, SiO2, has widespread applications ranging from optical components to refractory materials and is of geological importance as one of the major oxide components of the Earth's crust and mantle. The response of silica phases to dynamic loading has long been of interest for understanding the structural evolution of this fundamental oxide. Under shock compression both crystalline quartz and fused silica are characterized by the occurrence of a broad `mixed-phase region' (15-40 GPa) and a dense, high-pressure phase with much lower compressibility. Despite decades of study, the nature of this transformation and the identity of the high-pressure phase(s) remain poorly understood. In situ x-ray diffraction experiments on shock-compressed fused silica were conducted at the Dynamic Compression Sector of the Advanced Photon Source. The lattice-level structure was investigated through time-resolved x-ray diffraction measurements on samples reaching peak stress ranging from 12 to 47 GPa. Our results demonstrate that SiO2 adopts a dense amorphous structure in the `mixed-phase region' and abruptly transforms to stishovite above 34 GPa. These results provide clear evidence that high-pressure crystalline silicate phases can form from amorphous starting materials on the time-scale of laboratory shock experiments.

IN SITU SOURCE TREATMENT OF CR(VI) USING A FE(II)-BASED REDUCTANT BLEND: LONG-TERM MONITORING AND EVALUATION

EPA Science Inventory

The long-term effectiveness of a FeSO4 + Na2S2O4 reductant solution blend for in situ saturated zone treatment of dissolved and solid phase Cr(VI) in a high pH chromite ore processing solid waste (COPSW) fill material was investigated. Two field pilot injection studies were cond...

Optimizing of In Situ Bioremediation Technology to Manage Perchlorate-Contaminated Groundwater

DTIC Science & Technology

2003-03-01

template using the best fitness values. MOMGA then executes another cycle of initialization, primordial, and juxtapositional phases ( Van Veldhuizen ...Implementation of In Situ Remediation Technologies,” Journal of Contaminant Hydrology, 37(3): 295-317, 1999. Coello Coello, A. C., D.A. Van Veldhuizen , and G.B...Environmental Management. 56: 79-95, 1999. Van Veldhuizen , David A. Multiobjective Evolutionary Algorithms: Classifications, Analyses, and New

Watching Nanoscale Self-Assembly Kinetics of Gold Prisms in Liquids

NASA Astrophysics Data System (ADS)

Kim, Juyeong; Ou, Zihao; Jones, Matthew R.; Chen, Qian

We use liquid-phase transmission electron microscopy to watch self-assembly of gold triangular prisms into polymer-like structures. The in situ dynamics monitoring enabled by liquid-phase transmission electron microscopy, single nanoparticle tracking, and the marked conceptual similarity between molecular reactions and nanoparticle self-assembly combined elucidate the following mechanistic understanding: a step-growth polymerization based assembly statistics, kinetic pathways sampling particle curvature dependent energy minima and their interconversions, and directed assembly into polymorphs (linear or cyclic chains) through in situ modulation of the prism bonding geometry. Our study bridges the constituent kinetics on the molecular and nanoparticle length scales, which enriches the design rules in directed self-assembly of anisotropic nanoparticles.

Solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery mine, near Edgemont, South Dakota

USGS Publications Warehouse

Johnson, Raymond H.; Diehl, Sharon F.; Benzel, William M.

2013-01-01

This report releases solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery site near Edgemont, South Dakota. These cores were collected by Powertech Uranium Corporation, and material not used for their analyses were given to the U.S. Geological Survey for additional sampling and analyses. These additional analyses included total carbon and sulfur, whole rock acid digestion for major and trace elements, 234U/238U activity ratios, X-ray diffraction, thin sections, scanning electron microscopy analyses, and cathodoluminescence. This report provides the methods and data results from these analyses along with a short summary of observations.

Application of fluid-rock reaction studies to in situ recovery from oil sand deposits, Alberta, Canada - I. Aqueous phase results for an experimental-statistical study of water-bitumen-shale reactions

NASA Astrophysics Data System (ADS)

Boon, J. A.; Hitchon, Brian

1983-02-01

In situ recovery operations in oil sand deposits effectively represent man-imposed low to intermediate temperature metamorphism of the sediments in the deposit. In order to evaluate some of the reactions which occur, a factorial experiment was earned out in which a shale from the Lower Cretaceous McMurray Formation in the Athabasca oil sand deposit of Alberta, in the presence or absence of bitumen, was subjected to hydrothermal treatment with aqueous fluids of varying pH and salinity, at two different temperatures, for periods up to 92 hours. The aqueous fluid was analyzed and the analytical data subjected to statistical factor analysis and analysis of variance, which enabled identification of the main processes, namely, cation exchange, the production of two types of colloidal material, and the dissolution of quartz There is also saturation of the aqueous phase by. as yet unidentified, "total organic carbon" and complete conversion and removal of all nitrogen in the shale to the aqueous phase. These reactions have implications with regards to the economics of the in situ recovery process, specifically with respect to the reuse and/or disposal of the produced water and the plugging of the pore space and hence of reduction of permeability between the injection and production wells. As a result of these experiments it is suggested that monitoring of the composition of the produced water from in situ recovery operations in oil sand deposits would be advisable.

SERDP ER-1421 Abiotic and Biotic Mechanisms Controlling In Situ Remediation of NDMA: Final Report

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

Szecsody, James E.; McKinley, James P.; Crocker, Fiona H.

This laboratory-scale project was initiated to investigate in situ abiotic/biotic mineralization of NDMA. Under iron-reducing conditions, aquifer sediments showed rapid abiotic NDMA degradation to dimethylamine (DMA), nitrate, formate, and finally, CO2. These are the first reported experiments of abiotic NDMA mineralization. The NDMA reactivity of these different iron phases showed that adsorbed ferrous iron was the dominant reactive phase that promoted NDMA reduction, and other ferrous phases present (siderite, iron sulfide, magnetite, structural ferrous iron in 2:1 clays) did not promote NDMA degradation. In contrast, oxic sediments that were biostimulated with propane promoted biomineralization of NDMA by a cometabolic monooxygenasemore » enzyme process. Other monooxygenase enzyme processes were not stimulated with methane or toluene additions, and acetylene addition did not block mineralization. Although NDMA mineralization extent was the highest in oxic, biostimulated sediments (30 to 82%, compared to 10 to 26% for abiotic mineralization in reduced sediments), large 1-D column studies (high sediment/water ratio of aquifers) showed 5.6 times higher NDMA mineralization rates in reduced sediment (half-life 410 ± 147 h) than oxic biomineralization (half life 2293 ± 1866 h). Sequential reduced/oxic biostimulated sediment mineralization (half-life 3180 ± 1094 h) was also inefficient compared to reduced sediment. These promising laboratory-scale results for NDMA mineralization should be investigated at field scale. Future studies of NDMA remediation should focus on the comparison of this in situ abiotic NDMA mineralization (iron-reducing environments) to ex situ biomineralization, which has been shown successful in other studies.« less

Preparation and evaluation of injectable Rasagiline mesylate dual-controlled drug delivery system for the treatment of Parkinson's disease.

PubMed

Jiang, Ying; Zhang, Xuemei; Mu, Hongjie; Hua, Hongchen; Duan, Dongyu; Yan, Xiuju; Wang, Yiyun; Meng, Qingqing; Lu, Xiaoyan; Wang, Aiping; Liu, Wanhui; Li, Youxin; Sun, Kaoxiang

2018-11-01

A microsphere-gel in situ forming implant (MS-Gel ISFI) dual-controlled drug delivery system was applied to a high water-soluble small-molecule compound Rasagiline mesylate (RM) for effective treatment of Parkinson's disease. This injectable complex depot system combined an in situ phase transition gel with high drug-loading and encapsulation efficiency RM-MS prepared by a modified emulsion-phase separation method and optimized by Box-Behnken design. It was evaluated for in vitro drug release, in vivo pharmacokinetics, and in vivo pharmacodynamics. We found that the RM-MS-Gel ISFI system showed no initial burst release and had a long period of in vitro drug release (60 days). An in vivo pharmacokinetic study indicated a significant reduction (p < .01) in the initial high plasma drug concentration of the RM-MS-Gel ISFI system compared to that of the single RM-MS and RM-in situ gel systems after intramuscular injection to rats. A pharmacodynamic study demonstrated a significant reduction (p < .05) in 6-hydroxydopamine-induced contralateral rotation behavior and an effective improvement (p < .05) in dopamine levels in the striatum of the lesioned side after 28 days in animals treated with the RM-MS-Gel ISFI compared with that of animals treated with saline. MS-embedded in situ phase transition gel is superior for use as a biodegradable and injectable sustained drug delivery system with a low initial burst and long period of drug release for highly hydrophilic small molecule drugs.

In situ X-ray diffraction strain-controlled study of Ti–Nb–Zr and Ti–Nb–Ta shape memory alloys: crystal lattice and transformation features

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

Dubinskiy, S.; National University of Science and Technology “MISIS”, 4, Leninskiy prosp., Moscow 119049; Prokoshkin, S.

2014-02-15

Phase and structure transformations in biomedical Ti–21.8Nb–6.0Zr (TNZ) and Ti–19.7Nb–5.8Ta (TNT) shape memory alloys (at.%) under and without load in the − 150 to 100 °S temperature range are studied in situ using an original tensile module for a low-temperature chamber of an X-ray diffractometer. Alpha″- and beta-phase lattice parameters, the crystallographic resource of recovery strain, phase and structure transformation sequences, and microstress appearance and disappearance are examined, compared and discussed. For both alloys, the crystallographic resource of recovery strain decreases with temperature increase to become 4.5% for TNZ and 2.5% for TNT alloy (at RT). Loading at low temperaturesmore » leads to additional α″-phase formation and reorientation. Heating under load, as compared to strain-free heating, affects the reverse transformation sequence of both alloys in different ways. For TNZ alloy, strain-free heating results in simultaneous ω→β and α″→β transformations, whereas during heating under stress, they are sequential: β + ω→α″ precedes α″→β. For TNT alloy, strain-free heating results in reverse α″→β transformation, whereas during heating under stress, α″→β transformation is preceded by α″-phase reorientation. - Highlights: • Comparative in situ XRD analysis of Ti–Nb–Zr(Ta) shape memory alloys is realized. • Lattice parameters of β- and α″-phases are calculated in the − 150 to + 100 °C range. • The higher the temperature, the lower the α″→β transformation strain. • Loading at low temperatures results in α″-phase formation and reorientation. • Transformation sequences upon heating with and without loading are different.« less

In situ Mössbauer investigation of iron oxide catalyst in water gas shift reaction - Impact of oxyreduction potential and temperature

NASA Astrophysics Data System (ADS)

Cherkezova-Zheleva, Z.; Mitov, I.

2010-03-01

The aim of the study is to obtain the exact state of iron oxide catalyst active phase in reaction conditions, as well as the correlation between the active phase and catalytic properties of iron-containing catalysts. In situ Mössbauer spectroscopy is the major investigation technique. It is established that the change of reaction conditions (temperature and gas reaction mixture) lead to redistribution of the relative weight of spectra components and influence mainly tetrahedrally and octahedrally coordinated cations in Fe3O4 phase. It was concluded, that the active sites of the catalyst in studied reaction are probably pairs of Fe3++Fe2+-(Fe2.5+) ions, i.e. the mixed valance iron ions. The obtained catalytic activity can be explained with combination of the natural thermo-activated and catalytically induced electron exchange and better synchronizing of oxidation and reduction steps of the catalytic reaction.

High Zn Content Single-phase RS-MgZnO Suitable for Solar-blind Frequency Applications

NASA Astrophysics Data System (ADS)

Liang, H. L.; Mei, Z. X.; Liu, Z. L.; Guo, Y.; Azarov, A. Yu.; Kuznetsov, A. Yu.; Hallen, A.; Du, X. L.

2010-11-01

Single-phase rock-salt MgZnO films with high Zn content were successfully fabricated on the templates of MgO (111)/α-sapphire (0001) by radio-frequency plasma assisted molecular beam epitaxy. The influence of growth temperature on epitaxy of MgZnO alloy films was investigated by the combined studies of crystal structures, compositions, and optical properties. It is found that the incorporation of Zn atoms into the rock-salt MgZnO films is greatly enhanced at low temperature, confirmed by in-situ reflection high-energy electron diffraction observations and ex-situ X-ray diffraction characterization. Zn fraction in the single-phase rock-salt Mg0.53Zn0.47O film was determined by Rutherford backscattering spectrometry. Optical properties of the films were investigated by transmittance spectroscopy and reflectance spectroscopy, both of which demonstrate the solar-blind band gap and its dependence on Zn content.

Proposed in situ secondary ion mass spectrometry on Mars.

PubMed

Inglebert, R L; Klossa, B; Lorin, J C; Thomas, R

1995-01-01

Secondary ion mass spectrometry is a powerful analytical tool, which has the potentiality, through molecular ion emission, of detecting minor phases, as well as the unique capability of directly measuring isotope abundances in mineral or organic phases without any prior physical, chemical or thermal processing. Applied to the in situ analysis of the Martian regolith, it can provide evidence of the presence of carbonates and, by inference (if carbonates constitute significant deposits), of past liquid water--a necessary condition for the development of life. In addition, oxygen isotopic composition of carbonates preserves a record of the temperature at which this phase precipitated and may therefore help decipher the past climatology of Mars. Detection of a carbon isotopic composition shift between carbonates and organic matter (on Earth, the result of a kinetic fractionation effect during photosynthesis) would provide a definite clue regarding the existence of a past biochemical activity on Mars.

High strength, light weight Ti-Y composites and method of making same

DOEpatents

Verhoeven, John D.; Ellis, Timothy W.; Russell, Alan M.; Jones, Lawrence L.

1993-04-06

A high strength, light weight "in-situ" Ti-Y composite is produced by deformation processing a cast body having Ti and Y phase components distributed therein. The composite comprises elongated, ribbon-shaped Ti and Y phase components aligned along an axis of the deformed body.

High strength, light weight Ti-Y composites and method of making same

DOEpatents

Verhoeven, J.D.; Ellis, T.W.; Russell, A.M.; Jones, L.L.

1993-04-06

A high strength, light weight in-situ'' Ti-Y composite is produced by deformation processing a cast body having Ti and Y phase components distributed therein. The composite comprises elongated, ribbon-shaped Ti and Y phase components aligned along an axis of the deformed body.

In situ observation of quasimelting of diamond and reversible graphite-diamond phase transformations.

PubMed

Huang, J Y

2007-08-01

Because of technique difficulties in achieving the extreme high-pressure and high-temperature (HPHT) simultaneously, direct observation of the structures of carbon at extreme HPHT conditions has not been possible. Banhart and Ajayan discovered remarkably that carbon onions can act as nanoscopic pressure cells to generate high pressures. By heating carbon onions to approximately 700 degrees C and under electron beam irradiation, the graphite-to-diamond transformation was observed in situ by transmission electron microscopy (TEM). However, the highest achievable temperature in a TEM heating holder is less than 1000 degrees C. Here we report that, by using carbon nanotubes as heaters and carbon onions as high-pressure cells, temperatures higher than 2000 degrees C and pressures higher than 40 GPa were achieved simultaneously in carbon onions. At such HPHT conditions and facilitated by electron beam irradiation, the diamond formed in the carbon onion cores frequently changed its shape, size, orientation, and internal structure and moved like a fluid, implying that it was in a quasimelting state. The fluctuation between the solid phase of diamond and the fluid/amorphous phase of diamond-like carbon, and the changes of the shape, size, and orientation of the solid diamond, were attributed to the dynamic crystallization of diamond crystal from the quasimolten state and the dynamic graphite-diamond phase transformations. Our discovery offers unprecedented opportunities to studying the nanostructures of carbon at extreme conditions in situ and at an atomic scale.

Interaction potentials of anisotropic nanocrystals from the trajectory sampling of particle motion using in situ liquid phase transmission electron microscopy

DOE PAGES

Chen, Qian; Cho, Hoduk; Manthiram, Karthish; ...

2015-03-23

We demonstrate a generalizable strategy to use the relative trajectories of pairs and groups of nanocrystals, and potentially other nanoscale objects, moving in solution which can now be obtained by in situ liquid phase transmission electron microscopy (TEM) to determine the interaction potentials between nanocrystals. Such nanoscale interactions are crucial for collective behaviors and applications of synthetic nanocrystals and natural biomolecules, but have been very challenging to measure in situ at nanometer or sub-nanometer resolution. Here we use liquid phase TEM to extract the mathematical form of interaction potential between nanocrystals from their sampled trajectories. We show the power ofmore » this approach to reveal unanticipated features of nanocrystal–nanocrystal interactions by examining the anisotropic interaction potential between charged rod-shaped Au nanocrystals (Au nanorods); these Au nanorods assemble, in a tip-to-tip fashion in the liquid phase, in contrast to the well-known side-by-side arrangements commonly observed for drying-mediated assembly. These observations can be explained by a long-range and highly anisotropic electrostatic repulsion that leads to the tip-selective attachment. As a result, Au nanorods stay unassembled at a lower ionic strength, as the electrostatic repulsion is even longer-ranged. Our study not only provides a mechanistic understanding of the process by which metallic nanocrystals assemble but also demonstrates a method that can potentially quantify and elucidate a broad range of nanoscale interactions relevant to nanotechnology and biophysics.« less

Beamline Electrostatic Levitator (BESL) for in-situ High Energy K-Ray Diffraction Studies of Levitated Solids and Liquids at High Temperature

NASA Technical Reports Server (NTRS)

Gangopadhyay, A. K.; Lee, G. W.; Kelton, K. F.; Rogers, J. R.; Goldman, A. I.; Robinson, D. S.; Rathz, T. J.; Hyers, R. W.

2005-01-01

Determinations of the phase formation sequence, the crystal structures and the thermodynamic properties of materials at high temperatures are difficult because of contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic (EML), aerodynamic, and acoustic levitation, are most suitable these studies. An adaptation of ESL for in-situ structural studies of a wide range of materials, including metals, semiconductors, insulators using high energy (125 keV) synchrotron x-rays is described here. This beamline ESL (BESL) allows the in-situ determination of the atomic structures of equilibrium solid and liquid phases, including undercooled liquids, as well as real-time studies of solid-solid and liquid-solid phase transformations. The use of image plate (MAR345) or GE-Angio detectors enables fast (30 ms - 1s) acquisition of complete diffraction patterns over a wide q-range (4 - 140/mm). The wide temperature range (300 - 2500 K), containerless processing under high vacuum (10(exp -7) - 10(exp -8) torr), and fast data acquisition, make BESL particularly suitable for phase diagram studies of high temperature materials. An additional, critically important, feature of BESL is the ability to also make simultaneous measurement of a host of thermo-physical properties, including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension; all on the same sample and simultaneous with the structural measurements.

Probing microstructure and phase evolution of α-MoO 3 nanobelts for sodium-ion batteries by in situ transmission electron microscopy

DOE PAGES

Xia, Weiwei; Xu, Feng; Zhu, Chongyang; ...

2016-07-15

The fundamental electrochemical reaction mechanisms and the phase transformation pathways of layer-structured α-MoO 3 nanobelt during the sodiation/desodiation process to date remain largely unknown. In this study, to observe the real-time sodiation/desodiaton behaviors of α-MoO 3 during electrochemical cycling, we construct a MoO 3 anode sodium-ion battery inside a transmission electron microscope (TEM). Utilizing in situ TEM and electron diffraction pattern (EDP) observation, α-MoO 3 nanobelts are found to undergo a unique multi-step phase transformation. Upon the first sodiation, α-MoO 3 nanobelts initially form amorphous Na xMoO3 phase and are subsequently sodiated into intermediate phase of crystalline NaMoO 2, finallymore » resulting in the crystallized Mo nanograins embedded within the Na 2O matrix. During the first desodiation process, Mo nanograins are firstly re-oxidized into intermediate phase NaMoO 2 that is further transformed into amorphous Na 2MoO 3, resulting in an irreversible phase transformation. Upon subsequent sodiation/desodiation cycles, however, a stable and reversible phase transformation between crystalline Mo and amorphous Na2MoO 3 phases has been revealed. In conclusion, our work provides an in-deepth understanding of the phase transformation pathways of α-MoO 3 nanobelts upon electrochemical sodiation/desodiation processes, with the hope of assistance in designing sodium-ion batteries with enhanced performance.« less

Fatigue of LiNi0.8Co0.15Al0.05O2 in commercial Li ion batteries

NASA Astrophysics Data System (ADS)

Kleiner, Karin; Dixon, Ditty; Jakes, Peter; Melke, Julia; Yavuz, Murat; Roth, Christina; Nikolowski, Kristian; Liebau, Verena; Ehrenberg, Helmut

2015-01-01

The degradation of LiNi0.8Co0.15Al0.05O2 (LNCAO), a cathode material in lithium-ion-batteries, was studied using in situ powder diffraction and in situ Ni K edge X-ray absorption spectroscopy (XAS). The fatigued material was taken from a 7 Ah battery which was cycled for 34 weeks under defined durability conditions. Meanwhile, a cell was stored, as reference, under controlled conditions without electrochemical treatment. The fatigued LNCAO used in this study showed a capacity loss of 26% ± 9% compared to the non-cycled material. During charge and discharge the local and the overall structure of LNCAO was investigated by X-ray near edge structure (XANES) analysis, the extended X-ray absorption fine structure (EXAFS) analysis and by using Rietveld refinement of in situ powder diffraction patterns. Both powder diffraction and XAS revealed additional, rhombohedral phases which do not change with electrochemical cycling. Moreover, a phase with the lattice parameters of fully lithiated LNCAO was still present in the fatigued material at high potentials, while it was absent in the non-fatigued reference material. The coexistence of these phases is described by domains within the LNCAO particles, in correlation with the observed fatigue.

Evaluation of Methods for In-Situ Calibration of Field-Deployable Microphone Phased Arrays

NASA Technical Reports Server (NTRS)

Humphreys, William M.; Lockard, David P.; Khorrami, Mehdi R.; Culliton, William G.; McSwain, Robert G.

2017-01-01

Current field-deployable microphone phased arrays for aeroacoustic flight testing require the placement of hundreds of individual sensors over a large area. Depending on the duration of the test campaign, the microphones may be required to stay deployed at the testing site for weeks or even months. This presents a challenge in regards to tracking the response (i.e., sensitivity) of the individual sensors as a function of time in order to evaluate the health of the array. To address this challenge, two different methods for in-situ tracking of microphone responses are described. The first relies on the use of an aerial sound source attached as a payload on a hovering small Unmanned Aerial System (sUAS) vehicle. The second relies on the use of individually excited ground-based sound sources strategically placed throughout the array pattern. Testing of the two methods was performed in microphone array deployments conducted at Fort A.P. Hill in 2015 and at Edwards Air Force Base in 2016. The results indicate that the drift in individual sensor responses can be tracked reasonably well using both methods. Thus, in-situ response tracking methods are useful as a diagnostic tool for monitoring the health of a phased array during long duration deployments.

Effects of In Situ Intermetallics on the Microstructural Array and Saline Corrosion Performance of Cast Al/WCp Composites

NASA Astrophysics Data System (ADS)

Lekatou, A. G.; Gkikas, N.; Gousia, V.; Lentzaris, K.; Karantzalis, A. E.

2018-06-01

Al-matrix composites, ex situ reinforced with WC nanoparticles and in situ reinforced with Al3(Ti,W), Al12W, Al5W and Al4W, have been fabricated by casting assisted by K2TiF6 wetting agent addition and mechanical stirring. A satisfactory particle incorporation and distribution accompanied by a high reactivity have been attained. The presence, topography, chemical composition of all included phases and their occurrence as clusters or single particles are clarified and justified. Al12W is the predominant aluminide phase at WC ≤ 1.5 vol.%. Al4W (primarily) and Al5W (secondarily) are the predominant aluminide phases at WC ≥ 2.0 vol.%. WC nanoparticles have acted as heterogeneous nucleation sites to Al3Ti particles. Reverse polarization tests in 3.5 wt.% NaCl show that the governing form of corrosion is intergranular corrosion of Al around Al3FeSi2 eutectic, fine plates. The corrosion steps/mechanisms are identified. Clusters of aluminides and carbide nanoparticles, as well as intergranular WC nano-dispersoids and their Al-matrix have remained corrosion-free. The role of the aluminides combined with WC remaining nano-cores as inhibitors of the eutectic Al3FeSi2 cathodic activity is highlighted.

Development of High Strength Ni-Cu-Zr-Ti-Si-Sn In-Situ Bulk Metallic Glass Composites Reinforced by Hard B2 Phase

NASA Astrophysics Data System (ADS)

Park, Hyo Jin; Hong, Sung Hwan; Park, Hae Jin; Kim, Young Seok; Kim, Jeong Tae; Na, Young Sang; Lim, Ka Ram; Wang, Wei-Min; Kim, Ki Buem

2018-03-01

In the present study, the influence of atomic ratio of Zr to Ti on the microstructure and mechanical properties of Ni-Cu-Zr-Ti-Si-Sn alloys is investigated. The alloys were designed by fine replacement of Ti for Zr from Ni39Cu20Zr36-xTixSi2Sn3. The increase of Ti content enhances glass forming ability of the alloy by suppression of formation of (Ni, Cu)10(Zr, Ti)7 phase during solidification. With further increasing Ti content up to 24 at.%, the B2 phase is introduced in the amorphous matrix with a small amount of B19' phase from alloy melt. The bulk metallic glass composite containing B2 phase with a volume fraction of 10 vol% exhibits higher fracture strength ( 2.5 GPa) than that of monolithic bulk metallic glass ( 2.3 GPa). This improvement is associated to the individual mechanical characteristics of the B2 phase and amorphous matrix. The B2 phase exhibits higher hardness and modulus than those of amorphous matrix as well as effective stress accommodation up to the higher stress level than the yield strength of amorphous matrix. The large stress accommodation capacity of the hard B2 phase plays an important factor to improve the mechanical properties of in situ Ni-based bulk metallic glass composites.

Process for obtaining liquid fuel-oil and/or gaseous hydrocarbons from solid carbonaceous feed stocks

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

Hollaway, J.W.

1978-02-28

A process for forming a fuel-oil from coal is disclosed. The coal is treated in a low temperature carbonization retort to give coke, coal-gas and tar-oil. The coke is converted to water-gas which is then synthesized in a Fischer-Tropsch synthesizer to form fuel-oil. The tar-oil is hydrogenated in a hydro-treater by hydrogen produced from the coal-gas. Hydrogen is produced from coal-gas either in a thermal cracking chamber or by reforming the methane content to hydrogen and passing the resultant hydrogen/carbon monoxide mixture through a water-gas shift reactor and a carbon dioxide scrubber.

Using in situ synchrotron radiation wide angle X-ray scattering (WAXS) to study CaCO3 scale formation at ambient and elevated temperature.

PubMed

Chen, Tao; Neville, Anne; Sorbie, Ken; Zhong, Zhong

2007-01-01

The formation of calcium carbonate mineral scale is a persistent and expensive problem in oil and gas production, water piping systems, power generator, and batch precipitation. The aim of this paper is to further the understanding of scale formation and inhibition by in situ probing of crystal growth by synchrotron radiation wide angle X-ray scattering (WAXS) at ambient and elevated temperature. This novel technique enables in situ study of mineral scale formation and inhibition and as such, information on the nucleation and growth processes are accessible. This technique studies bulk precipitation and surface deposition in the same system and will be of great benefit to the understanding of an industrial scaling system. It offers an exciting prospect for the study of scaling. It has been shown that the nucleation and growth of various calcareous polymorphs and their individual crystal planes can be followed in real-time and from this the following conclusions are reached. The process of scale deposition on the surface can be divided into an unstable phase and a stable phase. The initial phase of crystallization of calcium carbonate is characterized by instability with individual planes from various vaterite and aragonite polymorphs emerging and subsequently disappearing under the hydrodynamic conditions. After the initial unstable phase, various calcium carbonate crystal planes adhere on the surface and then grow on the surface. At 25 degrees C, the main plane of surface deposit is calcite and a strong (104) peak is detected. The other calcite planes (102), (006), (110) (113) and (202) are hardly detectable under this condition. At 80 degrees C, the main planes in the surface deposit are the (104), (113) and (110) planes of calcite. Stable planes of vaterite and aragonite are also observed. This paper will discuss how surface scale evolves--exploring the power of the synchrotron in situ methodology.

Hydrolysis of polycarbonate in sub-critical water in fused silica capillary reactor with in situ Raman spectroscopy

USGS Publications Warehouse

Pan, Z.; Chou, I-Ming; Burruss, R.C.

2009-01-01

The advantages of using fused silica capillary reactor (FSCR) instead of conventional autoclave for studying chemical reactions at elevated pressure and temperature conditions were demonstrated in this study, including the allowance for visual observation under a microscope and in situ Raman spectroscopic characterization of polycarbonate and coexisting phases during hydrolysis in subcritical water.

Absorbable Gels for Modulated Bioavailability of Vaccines. Phase I

DTIC Science & Technology

1996-11-01

most of these devices were designed for repairing soft tissues , interest in using such transient devices, with or without biologically active components...potential applications of the in-situ-forming implants, and the more recent gel-formers, have been described to entail their use for tissue regeneration and...In Situ-Forming Biodegradable Polymeric Implants for Tissue Regeneration . Polym. Prepr., 35(2), 437 (1994). Edelman, R. et al, Immunization of

Lithiation Mechanism of Tunnel-Structured MnO 2 Electrode Investigated by In Situ Transmission Electron Microscopy

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

Lee, Seung-Yong; Wu, Lijun; Poyraz, Altug S.

Manganese oxide (α-MnO 2) has been considered as a promising energy material, including as a lithium-based battery electrode candidate, due to its environmental friendliness. Thanks to its unique 1D [2 × 2] tunnel structure, α-MnO 2 can be applied to a cathode by insertion reaction and to an anode by conversion reaction in corresponding voltage ranges, in a lithium-based battery. Numerous reports have attributed its remarkable performance to its unique tunnel structure; however, the precise electrochemical reaction mechanism remains unknown. In this study, finding of the lithiation mechanism of α-MnO 2 nanowire by in situ transmission electron microscopy (TEM) ismore » reported. By elaborately modifying the existing in situ TEM experimental technique, rapid lithium-ion diffusion through the tunnels is verified. Furthermore, by tracing the full lithiation procedure, the evolution of the MnO intermediate phase and the development of the MnO and Li 2O phases with preferred orientations is demonstrated, which explains how the conversion reaction occurs in α-MnO 2 material. This study provides a comprehensive understanding of the electrochemical lithiation process and mechanism of α-MnO 2 material, in addition to the introduction of an improved in situ TEM biasing technique.« less

Lithiation Mechanism of Tunnel-Structured MnO 2 Electrode Investigated by In Situ Transmission Electron Microscopy

DOE PAGES

Lee, Seung-Yong; Wu, Lijun; Poyraz, Altug S.; ...

2017-10-06

Manganese oxide (α-MnO 2) has been considered as a promising energy material, including as a lithium-based battery electrode candidate, due to its environmental friendliness. Thanks to its unique 1D [2 × 2] tunnel structure, α-MnO 2 can be applied to a cathode by insertion reaction and to an anode by conversion reaction in corresponding voltage ranges, in a lithium-based battery. Numerous reports have attributed its remarkable performance to its unique tunnel structure; however, the precise electrochemical reaction mechanism remains unknown. In this study, finding of the lithiation mechanism of α-MnO 2 nanowire by in situ transmission electron microscopy (TEM) ismore » reported. By elaborately modifying the existing in situ TEM experimental technique, rapid lithium-ion diffusion through the tunnels is verified. Furthermore, by tracing the full lithiation procedure, the evolution of the MnO intermediate phase and the development of the MnO and Li 2O phases with preferred orientations is demonstrated, which explains how the conversion reaction occurs in α-MnO 2 material. This study provides a comprehensive understanding of the electrochemical lithiation process and mechanism of α-MnO 2 material, in addition to the introduction of an improved in situ TEM biasing technique.« less

Mayenite Synthesized Using the Citrate Sol-Gel Method

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

Ude, Sabina N; Rawn, Claudia J; Meisner, Roberta A

2014-01-01

A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show themore » presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.« less

Visualization of structural evolution and phase distribution of a lithium vanadium oxide (Li 1.1V 3O 8) electrode via an operando and in situ energy dispersive X-ray diffraction technique

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

Zhang, Qing; Bruck, Andrea M.; Bock, David C.

We present Li 1+nV 3O 8 (n = 0–0.2) has been extensively investigated as a cathode material for Li ion batteries because of its superior electrochemical properties including high specific energy and good rate capability. In this paper, a synchrotron based energy dispersive X-ray diffraction (EDXRD) technique was employed to profile the phase transitions and the spatial phase distribution of a Li 1.1V 3O 8 electrode during electrochemical (de)lithiation in situ and operando. As annealing temperature during the preparation of the Li 1.1V 3O 8 material has a strong influence on the morphology and crystallinity, and consequently influences the electrochemicalmore » outcomes of the material, Li 1.1V 3O 8 materials prepared at two different temperatures, 500 and 300°C (LVO500 and LVO300), were employed in this study. The EDXRD spectra of LVO500 and LVO300 cells pre-discharged at C/18, C/40 and C/150 were recorded in situ, and phase localization and relative intensity of the peaks were compared. For cells discharged at the C/18 rate, although α and β phases were distributed uniformly within the LVO500 electrode, they were localized on two sides of the LVO300 electrode. Discharging rates of C/40 and C/150 led to homogeneous β phase formation in both LVO500 and LVO300 electrodes. Furthermore, the phase distribution as a function of position and (de)lithiation extent was mapped operando as the LVO500 cell was (de)lithiated. In conclusion, the operando data indicate that (1) the lithiation reaction initiated from the side of the electrode facing the Li anode and proceeded towards the side facing the steel can, (2) during discharge the phase transformation from a Li-poor to a Li-rich α phase and the formation of a β phase can proceed simultaneously in the electrode after the first formation of a β phase, and (3) the structural evolution occurring during charging is not the reverse of that during discharge and takes place homogenously throughout the electrode.« less

Visualization of structural evolution and phase distribution of a lithium vanadium oxide (Li 1.1V 3O 8) electrode via an operando and in situ energy dispersive X-ray diffraction technique

DOE PAGES

Zhang, Qing; Bruck, Andrea M.; Bock, David C.; ...

2017-05-03

We present Li 1+nV 3O 8 (n = 0–0.2) has been extensively investigated as a cathode material for Li ion batteries because of its superior electrochemical properties including high specific energy and good rate capability. In this paper, a synchrotron based energy dispersive X-ray diffraction (EDXRD) technique was employed to profile the phase transitions and the spatial phase distribution of a Li 1.1V 3O 8 electrode during electrochemical (de)lithiation in situ and operando. As annealing temperature during the preparation of the Li 1.1V 3O 8 material has a strong influence on the morphology and crystallinity, and consequently influences the electrochemicalmore » outcomes of the material, Li 1.1V 3O 8 materials prepared at two different temperatures, 500 and 300°C (LVO500 and LVO300), were employed in this study. The EDXRD spectra of LVO500 and LVO300 cells pre-discharged at C/18, C/40 and C/150 were recorded in situ, and phase localization and relative intensity of the peaks were compared. For cells discharged at the C/18 rate, although α and β phases were distributed uniformly within the LVO500 electrode, they were localized on two sides of the LVO300 electrode. Discharging rates of C/40 and C/150 led to homogeneous β phase formation in both LVO500 and LVO300 electrodes. Furthermore, the phase distribution as a function of position and (de)lithiation extent was mapped operando as the LVO500 cell was (de)lithiated. In conclusion, the operando data indicate that (1) the lithiation reaction initiated from the side of the electrode facing the Li anode and proceeded towards the side facing the steel can, (2) during discharge the phase transformation from a Li-poor to a Li-rich α phase and the formation of a β phase can proceed simultaneously in the electrode after the first formation of a β phase, and (3) the structural evolution occurring during charging is not the reverse of that during discharge and takes place homogenously throughout the electrode.« less

Thermal equation of state of MgSiO4H2 phase H determined by in situ X-ray diffraction and a multianvil apparatus

NASA Astrophysics Data System (ADS)

Nishi, Masayuki; Tsuchiya, Jun; Arimoto, Takeshi; Kakizawa, Sho; Kunimoto, Takehiro; Tange, Yoshinori; Higo, Yuji; Irifune, Tetsuo

2018-06-01

Phase H (MgSiO4H2) is the high-pressure form of dense hydrous silicate that could deliver surface water into the lower mantle. In this study, we determined the thermal equations of the state of phase H using in situ X-ray diffraction measurements, under conditions ranging from 34 to 62 GPa and 300 and 1300 K, using a multianvil apparatus. Analysis of the data, based on the Mie-Grüneisen-Debye model using third-order Burch-Murnaghan equations at a reference pressure of 35 GPa, yielded the following results V ref = 49.61 ± 0.01 Å3, K ref = 344.6±4.1 GPa, K_{{{ref}}}^' } = 3.05 ± 0.32, θ ref = 974 ± 146 K, γ ref = 1.8 ± 0.1, and q = 1.79 ± 0.55. The compressibility of phase H observed in this study agrees well with that derived from theoretical calculations in pressure regions where hydrogen bond symmetrization is predicted. It was also found that the volume and compressibility of phase H and δ-AlOOH were similar.

Significant increase of Curie temperature in nano-scale BaTiO{sub 3}

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

Li, Yueliang; Liao, Zhenyu; Fang, Fang

2014-11-03

The low Curie temperature (T{sub c} = 130 °C) of bulk BaTiO{sub 3} greatly limits its applications. In this work, the phase structures of BaTiO{sub 3} nanoparticles with sizes ranging from 2.5 nm to 10 nm were studied at various temperatures by using aberration-corrected transmission electron microscopy (TEM) equipped with an in-situ heating holder. The results implied that each BaTiO{sub 3} nanoparticle was composed of different phases, and the ferroelectric ones were observed in the shells due to the complicated surface structure. The ferroelectric phases in BaTiO{sub 3} nanoparticles remained at 600 °C, suggesting a significant increase of T{sub c}. Based on the in-situ TEM resultsmore » and the data reported by others, temperature-size phase diagrams for BaTiO{sub 3} particles and ceramics were proposed, showing that the phase transition became diffused and the T{sub c} obviously increased with decreasing size. The present work sheds light on the design and fabrication of advanced devices for high temperature applications.« less

Solid state amorphization of metastable Al 0.5TiZrPdCuNi high entropy alloy investigated by high voltage electron microscopy

DOE PAGES

Nagase, Takeshi; Takeuchi, Akira; Amiya, Kenji; ...

2017-07-18

Here, the phase stability of high entropy alloy (HEA), Al 0.5TiZrPdCuNi, under fast electron irradiation was studied by in-situ high voltage electron microscopy (HVEM). The initial phase of this alloy quenched from the melt was dependent on cooling rate. At high cooling rates an amorphous phase was obtained, whereas a body-centered cubic ( b.c.c.) phase were obtained at low cooling rates. By thermal crystallization of the amorphous phase b.c.c. phase nano-crystals were formed. Upon fast electron irradiation solid state amorphization (SSA) was observed in b.c.c. phase regardless of the initial microstructure (i.e., “coarse crystalline structure” or “nano-crystalline structure with grainmore » boundaries as a sink for point defects”). SSA behavior in the Al 0.5TiZrPdCuNi HEAs was investigated by in-situ transmission electron microscopy observations. Because the amorphization is very rarely achieved in a solid solution phase under fast electron irradiation in common metallic materials, this result suggests that the Al 0.5TiZrPdCuNi HEA from other common alloys and the other HEAs. The differences in phase stability against the irradiation between the Al 0.5TiZrPdCuNi HEA and the other HEAs were discussed. This is the first experimental evidence of SSA in HEAs stimulated by fast electron irradiation.« less

Effect of Extrusion Temperature on the Plastic Deformation of an Mg-Y-Zn Alloy Containing LPSO Phase Using In Situ Neutron Diffraction

NASA Astrophysics Data System (ADS)

Garces, G.; Perez, P.; Cabeza, S.; Kabra, S.; Gan, W.; Adeva, P.

2017-11-01

The evolution of the internal strains during in situ tension and compression tests has been measured in an MgY2Zn1 alloy containing long-period stacking ordered (LPSO) phase using neutron diffraction. The alloy was extruded at two different temperatures to study the influence of the microstructure and texture of the magnesium and the LPSO phases on the deformation mechanisms. The alloy extruded at 623 K (350 °C) exhibits a strong fiber texture with the basal plane parallel to the extrusion direction due to the presence of areas of coarse non-recrystallised grains. However, at 723 K (450 °C), the magnesium phase is fully recrystallised with grains randomly oriented. On the other hand, at the two extrusion temperatures, the LPSO phase orients their basal plane parallel to the extrusion direction. Yield stress is always slightly higher in compression than in tension. Independently on the stress sign and the extrusion temperature, the beginning of plasticity is controlled by the activation of the basal slip system in the dynamic recrystallized grains. Therefore, the elongated fiber-shaped LPSO phase which behaves as the reinforcement in a metal matrix composite is responsible for this tension-compression asymmetry.

Deformation and Phase Transformation Processes in Polycrystalline NiTi and NiTiHf High Temperature Shape Memory Alloys

NASA Technical Reports Server (NTRS)

Benafan, Othmane

2012-01-01

The deformation and transformation mechanisms of polycrystalline Ni49.9Ti50.1 and Ni50.3Ti29.7Hf20 (in at.%) shape memory alloys were investigated by combined experimental and modeling efforts aided by an in situ neutron diffraction technique at stress and temperature. The thermomechanical response of the low temperature martensite, the high temperature austenite phases, and changes between these two states during thermomechanical cycling were probed and reported. In the cubic austenite phase, stress-induced martensite, deformation twinning and slip processes were observed which helped in constructing a deformation map that contained the limits over which each of the identified mechanisms was dominant. Deformation of the monoclinic martensitic phase was also investigated where the microstructural changes (texture, lattice strains, and phase fractions) during room-temperature deformation and subsequent thermal cycling were compared to the bulk macroscopic response. When cycling between these two phases, the evolution of inelastic strains, along with the shape setting procedures were examined and used for the optimization of the transformation properties as a function of deformation levels and temperatures. Finally, this work was extended to the development of multiaxial capabilities at elevated temperatures for the in situ neutron diffraction measurements of shape memory alloys on the VULCAN Diffractometer at Oak Ridge National Laboratory.

Talbot-Lau x-ray deflectometry phase-retrieval methods for electron density diagnostics in high-energy density experiments.

PubMed

Valdivia, Maria Pia; Stutman, Dan; Stoeckl, Christian; Mileham, Chad; Begishev, Ildar A; Bromage, Jake; Regan, Sean P

2018-01-10

Talbot-Lau x-ray interferometry uses incoherent x-ray sources to measure refraction index changes in matter. These measurements can provide accurate electron density mapping through phase retrieval. An adaptation of the interferometer has been developed in order to meet the specific requirements of high-energy density experiments. This adaptation is known as a moiré deflectometer, which allows for single-shot capabilities in the form of interferometric fringe patterns. The moiré x-ray deflectometry technique requires a set of object and reference images in order to provide electron density maps, which can be costly in the high-energy density environment. In particular, synthetic reference phase images obtained ex situ through a phase-scan procedure, can provide a feasible solution. To test this procedure, an object phase map was retrieved from a single-shot moiré image obtained from a plasma-produced x-ray source. A reference phase map was then obtained from phase-stepping measurements using a continuous x-ray tube source in a small laboratory setting. The two phase maps were used to retrieve an electron density map. A comparison of the moiré and phase-stepping phase-retrieval methods was performed to evaluate single-exposure plasma electron density mapping for high-energy density and other transient plasma experiments. It was found that a combination of phase-retrieval methods can deliver accurate refraction angle mapping. Once x-ray backlighter quality is optimized, the ex situ method is expected to deliver electron density mapping with improved resolution. The steps necessary for improved diagnostic performance are discussed.

Kinetic control in the synthesis of metastable polymorphs: Bixbyite-to-Rh{sub 2}O{sub 3}(II)-to-corundum transition in In{sub 2}O{sub 3}

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

Bekheet, Maged F., E-mail: maged.bekheet@ceramics.tu-berlin.de; Fachgebiet Keramische Werkstoffe, Institut für Werkstoffwissenschaften und -technologien, Technische Universität Berlin, Hardenbergstraße 40, 10623 Berlin; Schwarz, Marcus R.

2015-09-15

An example for kinetic control of a solid-state phase transformation, in which the system evolves via the path with the lowest activation barrier rather than ending in the thermodynamically most favorable state, has been demonstrated. As a case study, the phase transitions of indium sesquioxide (In{sub 2}O{sub 3}) have been guided by theoretical calculations and followed in situ under high-pressure high-temperature conditions in multi-anvil assemblies. The corundum-type rh-In{sub 2}O{sub 3} has been synthesized from stable bixbyite-type c-In{sub 2}O{sub 3} in two steps: first generating orthorhombic Rh{sub 2}O{sub 3}-II-type o′-In{sub 2}O{sub 3} which is thermodynamically stable at 8.5 GPa/850 °C and,more » thereafter, exploiting the preferred kinetics in the subsequent transformation to the rh-In{sub 2}O{sub 3} during decompression. This synthesis strategy of rh-In{sub 2}O{sub 3} was confirmed ex situ in a toroid-type high-pressure apparatus at 8 GPa and 1100 °C. The pressure–temperature phase diagrams have been constructed and the stability fields of In{sub 2}O{sub 3} polymorphs and the crystallographic relationship between them have been discussed. - Graphical abstract: In situ energy-dispersive XRD patterns in multi-anvil assemblies show the sequence of phase transition c-In{sub 2}O{sub 3}→o′-In{sub 2}O{sub 3}→rh-In{sub 2}O{sub 3} under particular pressure and temperature conditions. The tick marks refer to the calculated Bragg positions of bixbyite-type (c-In{sub 2}O{sub 3}), Rh{sub 2}O{sub 3}-II-type (o–-In2O{sub 3}) and corundum-type (rh-In{sub 2}O{sub 3}). - Highlights: • The solid-state synthesis methods can be employed for obtaining metastable phases. • The phase transition of In{sub 2}O{sub 3} was guided by DFT calculations. • The phase transition of In{sub 2}O{sub 3} was followed in situ under HP–HT conditions. • Orthorhombic o′-In{sub 2}O{sub 3} polymorph was synthesized from c-In{sub 2}O{sub 3} at 8.5 GPa/850 °C. • Metastable rh-In{sub 2}O{sub 3} was obtained from o′-In{sub 2}O{sub 3} at 5.5 GPa during decompression.« less

Phase transition of aragonite in abalone nacre

NASA Astrophysics Data System (ADS)

An, Yuanlin; Liu, Zhiming; Wu, Wenjian

2013-04-01

Nacre is composed of about 95 vol.% aragonite and 5 vol.% biopolymer and famous for its "brick and mortar" microstructure. The phase transition temperature of aragonite in nacre is lower than the pure aragonite. In situ XRD was used to identify the phase transition temperature from aragonite to calcite in nacre, based on the analysis of TG-DSC of fresh nacre and demineralized nacre. The results indicate that the microstructure and biopolymer are the two main factors that influence the phase transition temperature of aragonite in nacre.

Room-Temperature Deformation and Martensitic Transformation of Two Co-Cr-Based Alloys

NASA Astrophysics Data System (ADS)

Cai, S.; Schaffer, J. E.; Huang, D.; Gao, J.; Ren, Y.

2018-05-01

Deformation of two Co-Cr alloys was studied by in situ synchrotron X-ray diffraction. Both alloys show stress-induced martensite transformation, which is affected by phase stabilities and transformation strains. Crystal structure of WC in Co-20Cr-15W-10Ni is identified. Compared with other phases present, it is elastically isotropic, exhibits high strength, and can elastically withstand strains exceeding 1 pct. Texture change during phase transformation is explained based on the crystal orientation relationship between γ- and ɛ-phases.

Demonstration of the AGI Universal Samplers (F.K.A. the GORE Modules) for Passive Sampling of Groundwater

DTIC Science & Technology

2014-03-27

Coefficient from Water into the Sorbent KOW Octanol-Water Partition Coefficient LF Low Flow LNAPL Light Non-aqueous Phase Liquid LTM Long-Term...Once in the vapor phase, the molecule can then diffuse through the mem- ERDC/CRREL TR-14-4 5 brane while liquid water is prevented from passing...remediation at this site was conducted in two phases. Phase I consisted of vertical contamina- tion profiling followed by the in situ injection of an