In Situ Observations of Thermoreversible Gelation and Phase Separation of Agarose and Methylcellulose Solutions under High Pressure.

PubMed

Kometani, Noritsugu; Tanabe, Masahiro; Su, Lei; Yang, Kun; Nishinari, Katsuyoshi

2015-06-04

Thermoreversible sol-gel transitions of agarose and methylcellulose (MC) aqueous solutions on isobaric cooling or heating under high pressure up to 400 MPa have been investigated by in situ observations of optical transmittance and falling-ball experiments. For agarose, which undergoes the gelation on cooling, the application of pressure caused a gradual rise in the cloud-point temperature over the whole pressure range examined, which is almost consistent with the pressure dependence of gelling temperature estimated by falling-ball experiments, suggesting that agarose gel is stabilized by compression and that the gelation occurs nearly in parallel with phase separation under ambient and high-pressure conditions. For MC, which undergoes the gelation on heating, the cloud-point temperature showed a slight rise with an initial elevation of pressure up to ∼150 MPa, whereas it showed a marked depression above 200 MPa. In contrast, the gelling temperature of MC, which is nearly identical to the cloud-point temperature at ambient pressure, showed a monotonous rise with increasing pressure up to 350 MPa, which means that MC undergoes phase separation prior to gelation on heating under high pressure above 200 MPa. Similar results were obtained for the melting process of MC gel on cooling. The unique behavior of the sol-gel transition of MC under high pressure has been interpreted in terms of the destruction of hydrophobic hydration by compression.

Atmospheric pressure spatial atomic layer deposition web coating with in situ monitoring of film thickness

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

Yersak, Alexander S.; Lee, Yung C.; Spencer, Joseph A.

Spectral reflectometry was implemented as a method for in situ thickness monitoring in a spatial atomic layer deposition (ALD) system. Al{sub 2}O{sub 3} films were grown on a moving polymer web substrate at 100 °C using an atmospheric pressure ALD web coating system, with film growth of 0.11–0.13 nm/cycle. The modular coating head design and the in situ monitoring allowed for the characterization and optimization of the trimethylaluminum and water precursor exposures, purge flows, and web speed. A thickness uniformity of ±2% was achieved across the web. ALD cycle times as low as 76 ms were demonstrated with a web speed of 1 m/smore » and a vertical gap height of 0.5 mm. This atmospheric pressure ALD system with in situ process control demonstrates the feasibility of low-cost, high throughput roll-to-roll ALD.« less

In situ Pressure Fluctuations of Polymer Melt Flow Instabilities: Experimental Evidence about their Origin and Dynamics.

PubMed

Palza, Humberto; Naue, Ingo F C; Wilhelm, Manfred

2009-11-02

Despite the practical importance of polymer melt instabilities, there is still a lack of experiments able to characterize in situ the origin and behavior of these phenomena. In this context, a new set-up consisting of high sensitive pressure transducers located inside a slit-die and an advanced mathematical framework to process in situ measurements of polymer melt instabilities, are developed and applied. Our results show for the first time that pressure oscillations can actually be detected inside the die under sharkskin conditions. This originates from a factor of 10(3) and 10(2) improvement in terms of time and pressure resolution. Furthermore, new evidence towards the propagation of the slip phenomena along the die in spurt instabilities are found. Copyright © 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sealed rotors for in situ high temperature high pressure MAS NMR

DOE PAGES

Hu, Jian Z.; Hu, Mary Y.; Zhao, Zhenchao; ...

2015-07-06

Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization,more » a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.« less

Sealed rotors for in situ high temperature high pressure MAS NMR

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

Hu, Jian Z.; Hu, Mary Y.; Zhao, Zhenchao

Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization,more » a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.« less

An in situ tribometer for measuring friction and wear of polymers in a high pressure hydrogen environment

NASA Astrophysics Data System (ADS)

Duranty, Edward R.; Roosendaal, Timothy J.; Pitman, Stan G.; Tucker, Joseph C.; Owsley, Stanley L.; Suter, Jonathan D.; Alvine, Kyle J.

2017-09-01

High pressure hydrogen effects on the friction and wear of polymers are of importance to myriad applications. Of special concern are those used in the infrastructure for hydrogen vehicle refueling stations, including compressor sliding seals, valves, and actuators. While much is known about potentially damaging embrittlement effects of hydrogen on metals, relatively little is known about the effects of high pressure hydrogen on polymers. However, based on the limited results that are published in the literature, polymers also apparently exhibit compatibility issues with hydrogen. An additional study is needed to elucidate these effects to avoid incompatibilities either through design or material selection. As part of this effort, we present here in situ high pressure hydrogen studies of the friction and wear on example polymers. To this end, we have built and demonstrated a custom-built pin-on-flat linear reciprocating tribometer and demonstrated its use with in situ studies of friction and wear behavior of nitrile butadiene rubber polymer samples in 28 MPa hydrogen. Tribology results indicate that friction and wear is increased in high pressure hydrogen as compared both with values measured in high pressure argon and ambient air conditions.

In Situ XANES of U and Th in Silicate Liquids at High Pressure and Temperature

NASA Astrophysics Data System (ADS)

Mallmann, G.; Wykes, J.; Berry, A.; O'Neill, H. S.; Cline, C. J., II; Turner, S.; Rushmer, T. A.

2016-12-01

Although the chemical environments of elements in silicate melts at specific conditions of temperature, pressure and oxygen fugacity (fO2) are often inferred from measurements after quenching the melts to glasses, it is widely recognized that changes may occur during the quenching process, making measurements in situ at high pressure and temperature highly desirable. A case of importance in geochemistry is the speciation of uranium in silicate melts as a function of pressure. Evidence from mineral-melt partitioning and XANES (X-ray Absorption Near-Edge Structure) spectroscopy of glasses suggests that U5+ may be stable at low pressures in the Earth's crust (along with U4+ or U6+, depending on fO2) where basaltic liquids crystallize, but not in the Earth's upper mantle where peridotite partially melts to produce such liquids. To test these observations we recorded in situ transmission U and Th L3-edge XANES spectra of U and Th-doped silicate liquids at 1.6 GPa and 1350°C using the D-DIA apparatus at the X-ray Absorption Spectroscopy Beamline of the Australian Synchrotron. Data for thorium, which occurs exclusively as a tetravalent cation under terrestrial fO2 conditions, were collected as a `control' to monitor for changes in coordination. The cell assembly consisted of a boron-epoxy cube as pressure medium, alumina sleeve and cylindrical graphite heater. The starting mix, a powdered synthetic average MORB silicate glass doped with 2 wt.% of U and Th, was loaded into San Carlos olivine capsules along with solid oxygen buffers (either Re-ReO2 or Ru-RuO2) in a sandwich arrangement. The capsule was then placed inside the graphite heater and insulated with crushable MgO powder. Temperature was monitored using a type D thermocouple. U and Th L3-edge XANES spectra were recorded throughout the heating/compression cycle and then after quenching. Our preliminary assessment indicates that the U-XANES spectra recorded for the liquid in situ at high pressure and temperature and

Determining pH at elevated pressure and temperature using in situ ¹³C NMR.

PubMed

Surface, J Andrew; Wang, Fei; Zhu, Yanzhe; Hayes, Sophia E; Giammar, Daniel E; Conradi, Mark S

2015-02-03

We have developed an approach for determining pH at elevated pressures and temperatures by using (13)C NMR measurements of inorganic carbon species together with a geochemical equilibrium model. The approach can determine in situ pH with precision better than 0.1 pH units at pressures, temperatures, and ionic strengths typical of geologic carbon sequestration systems. A custom-built high pressure NMR probe was used to collect (13)C NMR spectra of (13)C-labeled CO2 reactions with NaOH solutions and Mg(OH)2 suspensions at pressures up to 107 bar and temperatures of 80 °C. The quantitative nature of NMR spectroscopy allows the concentration ratio [CO2]/[HCO3(-)] to be experimentally determined. This ratio is then used with equilibrium constants calculated for the specific pressure and temperature conditions and appropriate activity coefficients for the solutes to calculate the in situ pH. The experimentally determined [CO2]/[HCO3(-)] ratios agree well with the predicted values for experiments performed with three different concentrations of NaOH and equilibration with multiple pressures of CO2. The approach was then applied to experiments with Mg(OH)2 slurries in which the change in pH could track the dissolution of CO2 into solution, rapid initial Mg(OH)2 dissolution, and onset of magnesium carbonate precipitation.

Mechanism of Particle Formation in Silver/Epoxy Nanocomposites Obtained through a Visible-Light-Assisted in Situ Synthesis.

PubMed

dell'Erba, Ignacio E; Martínez, Francisco D; Hoppe, Cristina E; Eliçabe, Guillermo E; Ceolín, Marcelo; Zucchi, Ileana A; Schroeder, Walter F

2017-10-03

A detailed understanding of the processes taking place during the in situ synthesis of metal/polymer nanocomposites is crucial to manipulate the shape and size of nanoparticles (NPs) with a high level of control. In this paper, we report an in-depth time-resolved analysis of the particle formation process in silver/epoxy nanocomposites obtained through a visible-light-assisted in situ synthesis. The selected epoxy monomer was based on diglycidyl ether of bisphenol A, which undergoes relatively slow cationic ring-opening polymerization. This feature allowed us to access a full description of the formation process of silver NPs before this was arrested by the curing of the epoxy matrix. In situ time-resolved small-angle X-ray scattering investigation was carried out to follow the evolution of the number and size of the silver NPs as a function of irradiation time, whereas rheological experiments combined with near-infrared and ultraviolet-visible spectroscopies were performed to interpret how changes in the rheological properties of the matrix affect the nucleation and growth of particles. The analysis of the obtained results allowed us to propose consistent mechanisms for the formation of metal/polymer nanocomposites obtained by light-assisted one-pot synthesis. Finally, the effect of a thermal postcuring treatment of the epoxy matrix on the particle size in the nanocomposite was investigated.

Compensating for pneumatic distortion in pressure sensing devices

NASA Technical Reports Server (NTRS)

Whitmore, Stephen A.; Leondes, Cornelius T.

1990-01-01

A technique of compensating for pneumatic distortion in pressure sensing devices was developed and verified. This compensation allows conventional pressure sensing technology to obtain improved unsteady pressure measurements. Pressure distortion caused by frictional attenuation and pneumatic resonance within the sensing system makes obtaining unsteady pressure measurements by conventional sensors difficult. Most distortion occurs within the pneumatic tubing which transmits pressure impulses from the aircraft's surface to the measurement transducer. To avoid pneumatic distortion, experiment designers mount the pressure sensor at the surface of the aircraft, (called in-situ mounting). In-situ transducers cannot always fit in the available space and sometimes pneumatic tubing must be run from the aircraft's surface to the pressure transducer. A technique to measure unsteady pressure data using conventional pressure sensing technology was developed. A pneumatic distortion model is reduced to a low-order, state-variable model retaining most of the dynamic characteristics of the full model. The reduced-order model is coupled with results from minimum variance estimation theory to develop an algorithm to compensate for the effects of pneumatic distortion. Both postflight and real-time algorithms are developed and evaluated using simulated and flight data.

An Insertable Passive LC Pressure Sensor Based on an Alumina Ceramic for In Situ Pressure Sensing in High-Temperature Environments.

PubMed

Xiong, Jijun; Li, Chen; Jia, Pinggang; Chen, Xiaoyong; Zhang, Wendong; Liu, Jun; Xue, Chenyang; Tan, Qiulin

2015-08-31

Pressure measurements in high-temperature applications, including compressors, turbines, and others, have become increasingly critical. This paper proposes an implantable passive LC pressure sensor based on an alumina ceramic material for in situ pressure sensing in high-temperature environments. The inductance and capacitance elements of the sensor were designed independently and separated by a thermally insulating material, which is conducive to reducing the influence of the temperature on the inductance element and improving the quality factor of the sensor. In addition, the sensor was fabricated using thick film integrated technology from high-temperature materials that ensure stable operation of the sensor in high-temperature environments. Experimental results showed that the sensor accurately monitored pressures from 0 bar to 2 bar at temperatures up to 800 °C. The sensitivity, linearity, repeatability error, and hysteretic error of the sensor were 0.225 MHz/bar, 95.3%, 5.5%, and 6.2%, respectively.

In Situ Observation of Gypsum-Anhydrite Transition at High Pressure and High Temperature

NASA Astrophysics Data System (ADS)

Liu, Chuan-Jiang; Zheng, Hai-Fei

2012-04-01

An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC). The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 MPa. With increasing temperature, the anhydrite (CaSO4) phase precipitates at 250-320°C in the pressure range of 1.0-1.5GPa, indicating that under a saturated water condition, both stable conditions of pressure and temperature and high levels of Ca and SO4 ion concentrations in aqueous solution are essential for the formation of anhydrite. A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(GPa) = 0.0068T-0.7126 (250°C<=T<=320°C). Anhydrite remained stable during rapid cooling of the sample chamber, showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is irreversible at high pressure and high temperature.

N-isopropylacrylamide-based fine-dispersed thermosensitive ferrogels obtained via in-situ technique.

PubMed

Korotych, O; Samchenko, Yu; Boldeskul, I; Ulberg, Z; Zholobak, N; Sukhodub, L

2013-03-01

Thermosensitive hydrogels with magnetic properties (ferrogels) are very promising for medical application, first of all, for the design of targeted delivery systems with controlled release of drugs and for magnetic hyperthermia and chemotherapy treatment of cancer. These magnetic hydrogels could be obtained using diverse techniques: ex- and in-situ syntheses. The present work is devoted to the study of magnetite (Fe(3)O(4)) formation inside the nanoreactors of (co)polymeric hydrogels. Polymeric templates (hydrogel films and fine-dispersed hydrogels) used for obtaining ferrogels were based on acrylic monomers: thermosensitive N-isopropylacrylamide, and hydrophilic acrylamide. Covalent cross-linking was accomplished using bifunctional monomer N,N'-methylenebisacrylamide. Influence of hydrophilic-lipophilic balance of polymeric templates and concentration of iron cations on the magnetite formation were investigated along with the development of ferrogel preparation technique. Cytotoxicity, physical and chemical properties of obtained magnetic hydrogels have been studied in this work. Copyright © 2012 Elsevier B.V. All rights reserved.

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

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

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

DOE PAGES

Meng, Yue; Hrubiak, Rostislav; Rod, Eric; ...

2015-07-17

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

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

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areasmore » including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

A New Technique for In Situ X-ray Microtomography Under High Pressure

NASA Astrophysics Data System (ADS)

Uchida, T.; Wang, Y.; Westferro, F.; Gebhardt, J.; Rivers, M. L.; Sutton, S. R.

2004-12-01

We have developed a new technique for in situ synchrotron microtomography to study texture evolution in multi-phase specimens under high pressure and temperature. Two critical issues in performing tomography experiments under pressure are (1) the limited X-ray access to the sample because of the highly absorbing materials, such as tungsten carbide and tool steel, typically used in the pressure vessel and (2) a high pressure compatible rotation mechanism to collect projections of the sample continuously from 0 to 180° . We addressed these issues by (1) employing an opposed-anvil high pressure cell, known as the Drickamer cell, with an X-ray transparent containment ring, to allow panoramic X-ray access, and (2) rotating the Dricakmer cell by Harmonic DriveTM gear reducers, with thrust bearings supporting the hydraulic load. The design of the rotation mechanism benefited from the rotational deformation apparatus developed by Yamazaki and Karato (Rev. Sci. Instrum., 72, 4207, 2001). We report results obtained from a test run performed under pressure with monochromatic synchrotron radiation. A sapphire sphere (1.0 mm dia.) was embedded in a powdered mixture of Fe and 9 wt.% S alloy. The diameter of the sample chamber was 2 mm. Under pressure, the entire Drickamer cell was rotated to collect radiographs of the sample at various angles from 0 to 179.5° in 0.5° step size. Computational reconstruction of these projections provided three dimensional (3D) distribution of linear attenuation coefficient of the sample with a spatial resolution of 6 microns. The shape change in the sapphire sphere during compression was clearly observed. Using the program Blob3d, reconstructed 3D images of the sphere were separated from the surrounding Fe-S alloy. Volumes of the sphere were then accurately determined from the extracted images, by carefully defining the image intensity threshold. The errors in the volume measurement are about 0.3 to 0.7%, mostly due to shadowing by anvil

In situ structural analysis of calcium aluminosilicate glasses under high pressure.

PubMed

Muniz, R F; de Ligny, D; Martinet, C; Sandrini, M; Medina, A N; Rohling, J H; Baesso, M L; Lima, S M; Andrade, L H C; Guyot, Y

2016-08-10

In situ micro-Raman spectroscopy was used to investigate the structural evolution of OH(-)-free calcium aluminosilicate glasses, under high pressure and at room temperature. Evaluation was made of the role of the SiO2 concentration in percalcic join systems, for Al/(Al  +  Si) in the approximate range from 0.9 to 0.2. Under high pressure, the intensity of the main band related to the bending mode of bridging oxygen ([Formula: see text][T-O-T], where T  =  Si or Al) decreased gradually, suggesting that the bonds were severely altered or even destroyed. In Si-rich glasses, compression induced a transformation of Q (n) species to Q (n-1). In the case of Al-rich glass, the Al in the smallest Q (n) units evolved from tetrahedral to higher-coordinated Al (([5])Al and ([6])Al). Permanent structural changes were observed in samples recovered from the highest pressure of around 15 GPa and, particularly for Si-rich samples, the recovered structure showed an increase of three-membered rings in the Si/Al tetrahedral network.

An Insertable Passive LC Pressure Sensor Based on an Alumina Ceramic for In Situ Pressure Sensing in High-Temperature Environments

PubMed Central

Xiong, Jijun; Li, Chen; Jia, Pinggang; Chen, Xiaoyong; Zhang, Wendong; Liu, Jun; Xue, Chenyang; Tan, Qiulin

2015-01-01

Pressure measurements in high-temperature applications, including compressors, turbines, and others, have become increasingly critical. This paper proposes an implantable passive LC pressure sensor based on an alumina ceramic material for in situ pressure sensing in high-temperature environments. The inductance and capacitance elements of the sensor were designed independently and separated by a thermally insulating material, which is conducive to reducing the influence of the temperature on the inductance element and improving the quality factor of the sensor. In addition, the sensor was fabricated using thick film integrated technology from high-temperature materials that ensure stable operation of the sensor in high-temperature environments. Experimental results showed that the sensor accurately monitored pressures from 0 bar to 2 bar at temperatures up to 800 °C. The sensitivity, linearity, repeatability error, and hysteretic error of the sensor were 0.225 MHz/bar, 95.3%, 5.5%, and 6.2%, respectively. PMID:26334279

Reliability of cystometrically obtained intravesical pressures in patients with neurogenic bladders.

PubMed

Hess, Marika J; Lim, Lance; Yalla, Subbarao V

2002-01-01

Urodynamic studies in patients with neurogenic bladder detect and categorize neurourodynamic states, identify the risk for urologic sequelae, and determine the necessity for interventions. Because urodynamic studies serves as a prognostic indicator and guides patient management, pressure measurements during the study must accurately represent bladder function under physiologic conditions. Because nonphysiologic bladder filling used during conventional urodynamic studies may alter the bladder's accommodative properties, we studied how closely the intravesical pressures obtained before filling cystometry resembled those obtained during the filling phase of the cystometrogram. Twenty-two patients (21 men, 1 woman) with neurogenic bladders underwent standard urodynamic studies. A 16F triple-lumen catheter was inserted into the bladder, and the intravesical pressures were recorded (physiologic volume-specific pressures, PVSP). After emptying the bladder, an equal volume of normal saline solution was reinfused, and the pressures were recorded again (cystometric volume-specific pressure, CVSP). All patients underwent routine fluoroscopically assisted urodynamic testing. The PVSP and the CVSP were compared using the Wilcoxon signed ranks test. P value of .05 was significant. The mean PVSP was 14.5 cmH2O (range, 4-42 cmH2O) and mean CVSP was 20.6 cmH2O (range, 6-70 cmH2O). The CVSP was significantly higher than the PVSP (P = .01). Filling pressures during cystometry (CVSP) were significantly higher than the pressures measured at rest (PVSP). This study also suggests a strong correlation between PVSP and CVSP.

Pressure-induced amorphization and reactivity of solid dimethyl acetylene probed by in situ FTIR and Raman spectroscopy

NASA Astrophysics Data System (ADS)

Guan, Jiwen; Daljeet, Roshan; Kieran, Arielle; Song, Yang

2018-06-01

Conjugated polymers are prominent semiconductors that have unique electric conductivity and photoluminescence. Synthesis of conjugated polymers under high pressure is extremely appealing because it does not require a catalyst or solvent used in conventional chemical methods. Transformation of acetylene and many of its derivatives to conjugated polymers using high pressure has been successfully achieved, but not with dimethyl acetylene (DMA). In this work, we present a high-pressure study on solid DMA using a diamond anvil cell up to 24.4 GPa at room temperature characterized by in situ Fourier transform infrared and Raman spectroscopy. Our results show that solid DMA exists in a phase II crystal structure and is stable up to 12 GPa. Above this pressure, amorphization was initiated and the process was completed at 24.4 GPa. The expected polymeric transformation was not evident upon compression, but only observed upon decompression from a threshold compression pressure (e.g. 14.4 GPa). In situ florescence measurements suggest excimer formation via crystal defects, which induces the chemical reactions. The vibrational spectral analysis suggests the products contain the amorphous poly(DMA) and possibly additional amorphous hydrogenated carbon material.

Pressure-induced amorphization and reactivity of solid dimethyl acetylene probed by in situ FTIR and Raman spectroscopy.

PubMed

Guan, Jiwen; Daljeet, Roshan; Kieran, Arielle; Song, Yang

2018-06-06

Conjugated polymers are prominent semiconductors that have unique electric conductivity and photoluminescence. Synthesis of conjugated polymers under high pressure is extremely appealing because it does not require a catalyst or solvent used in conventional chemical methods. Transformation of acetylene and many of its derivatives to conjugated polymers using high pressure has been successfully achieved, but not with dimethyl acetylene (DMA). In this work, we present a high-pressure study on solid DMA using a diamond anvil cell up to 24.4 GPa at room temperature characterized by in situ Fourier transform infrared and Raman spectroscopy. Our results show that solid DMA exists in a phase II crystal structure and is stable up to 12 GPa. Above this pressure, amorphization was initiated and the process was completed at 24.4 GPa. The expected polymeric transformation was not evident upon compression, but only observed upon decompression from a threshold compression pressure (e.g. 14.4 GPa). In situ florescence measurements suggest excimer formation via crystal defects, which induces the chemical reactions. The vibrational spectral analysis suggests the products contain the amorphous poly(DMA) and possibly additional amorphous hydrogenated carbon material.

In situ modification of chromatography adsorbents using cold atmospheric pressure plasmas

NASA Astrophysics Data System (ADS)

Olszewski, P.; Willett, T. C.; Theodosiou, E.; Thomas, O. R. T.; Walsh, J. L.

2013-05-01

Efficient manufacturing of increasingly sophisticated biopharmaceuticals requires the development of new breeds of chromatographic materials featuring two or more layers, with each layer affording different functions. This letter reports the in situ modification of a commercial beaded anion exchange adsorbent using atmospheric pressure plasma generated within gas bubbles. The results show that exposure to He-O2 plasma in this way yields significant reductions in the surface binding of plasmid DNA to the adsorbent exterior, with minimal loss of core protein binding capacity; thus, a bi-layered chromatography material exhibiting both size excluding and anion exchange functionalities within the same bead is produced.

Laboratory evaluation of the Level TROLL 100 manufactured by In-Situ Inc.: results of pressure and temperature tests

USGS Publications Warehouse

Carnley, Mark V.; Fulford, Janice M.; Brooks, Myron H.

2013-01-01

The Level TROLL 100 manufactured by In-Situ Inc. was evaluated by the U.S. Geological Survey (USGS) Hydrologic Instrumentation Facility (HIF) for conformance to the manufacturer’s accuracy specifications for measuring pressure throughout the device’s operating temperature range. The Level TROLL 100 is a submersible, sealed, water-level sensing device with an operating pressure range equivalent to 0 to 30 feet of water over a temperature range of −20 to 50 degrees Celsius (°C). The device met the manufacturer’s stated accuracy specifications for pressure within its temperature-compensated operating range of 0 to 50 °C. The device’s accuracy specifications did not meet established USGS requirements for primary water-stage sensors used in the operation of streamgages, but the Level TROLL 100 may be suitable for other hydrologic data-collection applications. As a note, the Level TROLL 100 is not designed to meet USGS accuracy requirements. Manufacturer accuracy specifications were evaluated, and the procedures followed and the results obtained are described in this report. USGS accuracy requirements are routinely examined and reported when instruments are evaluated at the HIF.

In situ investigation of Geobacillus stearothermophilus spore germination and inactivation mechanisms under moderate high pressure.

PubMed

Georget, Erika; Kapoor, Shobhna; Winter, Roland; Reineke, Kai; Song, Youye; Callanan, Michael; Ananta, Edwin; Heinz, Volker; Mathys, Alexander

2014-08-01

Bacterial spores are a major concern for food safety due to their high resistance to conventional preservation hurdles. Innovative hurdles can trigger bacterial spore germination or inactivate them. In this work, Geobacillus stearothermophilus spore high pressure (HP) germination and inactivation mechanisms were investigated by in situ infrared spectroscopy (FT-IR) and fluorometry. G. stearothermophilus spores' inner membrane (IM) was stained with Laurdan fluorescent dye. Time-dependent FT-IR and fluorescence spectra were recorded in situ under pressure at different temperatures. The Laurdan spectrum is affected by the lipid packing and level of hydration, and provided information on the IM state through the Laurdan generalized polarization. Changes in the -CH2 and -CH3 asymmetric stretching bands, characteristic of lipids, and in the amide I' band region, characteristic of proteins' secondary structure elements, enabled evaluation of the impact of HP on endospores lipid and protein structures. These studies were complemented by ex situ analyses (plate counts and microscopy). The methods applied showed high potential to identify germination mechanisms, particularly associated to the IM. Germination up to 3 log10 was achieved at 200 MPa and 55 °C. A molecular-level understanding of these mechanisms is important for the development and validation of multi-hurdle approaches to achieve commercial sterility. Copyright © 2014 Elsevier Ltd. All rights reserved.

Low-pressure chemical vapor deposition of low in situ phosphorus doped silicon thin films

NASA Astrophysics Data System (ADS)

Sarret, M.; Liba, A.; Bonnaud, O.

1991-09-01

In situ low phosphorus doped silicon films are deposited onto glass substrates by low-pressure chemical vapor deposition method. The deposition parameters, temperature, total pressure, and pure silane gas flow are, respectively, fixed at 550 °C, 0.08 Torr, and 50 sccm. The varying deposition parameter is phosphine/silane mole ratio; when this ratio varies from 2×10-6 to 4×10-4, the phosphorus concentration and the resistivity after annealing, respectively, vary from 2×1018 to 3×1020 atoms cm-3 and from 1.5 Ω cm to 2.5×10-3 Ω cm.

Fixation of CO 2 by chrysotile in low-pressure dry and moist carbonation: Ex-situ and in-situ characterizations

NASA Astrophysics Data System (ADS)

Larachi, Faïçal; Daldoul, Insaf; Beaudoin, Georges

2010-06-01

A detailed study of low-pressure gas-solid carbonation of chrysotile in dry and humid environments has been carried out. The evolving structure of chrysotile and its reactivity as a function of temperature (300-1200 °C), humidity (0-10 mol %) and CO 2 partial pressure (20-67 mol %), thermal preconditioning, and alkali metal doping (Li, Na, K, Cs) have been monitored through in-situ X-ray photoelectron spectroscopy, isothermal thermogravimetry/mass spectrometry, ex-situ X-ray powder diffraction, and water and nitrogen adsorption/desorption. Based on chrysotile crystalline structure and its nanofibrilar orderliness, a multistep carbonation mechanism was elaborated to explain the role of water during chrysotile partial amorphisation, formation of periclase, brucite, and hydromagnesite crystalline phases, and surface passivation thereof, during humid carbonation. The weak carbonation reactivity was rationalized in terms of incongruent CO 2 van der Waals molecular diameters with the octahedral-tetrahedral lattice constants of chrysotile. This lack of reactivity appeared to be relatively indifferent to the facilitated water crisscrossing during chrysotile core dehydroxylation/pseudo-amorphisation and surface hydroxylation induced product stabilization during humid carbonation. Thermodynamic stability domains of the species observed at low pressure have been thoroughly discussed on the basis of X-ray powder diffraction patterns and X-ray photoelectron spectroscopy evidence. The highest carbon dioxide uptake occurred at 375 °C in moist atmospheres. On the basis of chrysotile fresh N 2 BET area, nearly 15 atoms out of 100 of the surface chrysotile brucitic Mg moiety have been carbonated at this temperature which was tantamount to the carbonation of about 2.5 at. % of the total brucitic Mg moiety in chrysotile. The carbonation of brucite (Mg(OH) 2) impurities coexisting in chrysotile was minor and estimated to contribute by less than 17.6 at. % of the total converted

New results of the post-spinel transition pressure in Mg2SiO4 by means of in-situ X-ray diffraction in a multi-anvil press: complete agreement with the 660-km discontinuity depth

NASA Astrophysics Data System (ADS)

Ishii, T.; Huang, R.; Fei, H.; Koemets, I.; Liu, Z.; Maeda, F.; Yuan, L.; Wang, L.; Druzhbin, D.; Yamamoto, T.; Bhat, S.; Farla, R. J.; Kawazoe, T.; Tsujino, N.; Kulik, E.; Higo, Y.; Tange, Y.; Katsura, T.

2017-12-01

It has been accepted that the 660-km discontinuity (D660) is caused by the post-spinel (Psp) transition, which is decomposition of ringwoodite (Rw) to bridgmanite (Brg) + ferropericlase. Nevertheless, all of in-situ X-ray diffraction studies with multi-anvil presses (MAP) gave distinctively lower transition pressures than that of the D660 (23.4 GPa). Although Fei et al. (2004) claimed that their Psp transition pressure explains the D660, it is still 0.5 GPa lower by considering the geotherm. If these results were accepted, the Psp would not account for the D660. In this study, we re-investigated the Psp transition pressure in Mg2SiO4 by in-situ X-ray diffraction using a MAP. A fine-grained mixture of forsterite, enstatite and periclase (Pc) and an MgO pressure marker were placed at the center of a furnace. The sample was compressed to 6-7 MN and heated to 1100 K to synthesize a mixture of Rw, akimotoite and Pc. After that, more press load was applied to obtain sample pressures of ca. 23 GPa, and the sample was then heated to 1700 K, keeping this temperature for 1-2 hours. During keeping the temperature, the press load was first rapidly, and then gradually increased to prevent pressure drop. Phase identification and pressure determination were conducted with alternatively accumulated diffraction patterns of the sample and pressure maker. We bracketed the transition pressures by 23.7 and 24.0 GPa at 1700 K based on the third-order Birch-Murnaghan and Vinet EOSs of MgO given by Tange et al. (2009), respectively. The transition pressure at 2000 K is estimated to be 23.2-23.5 GPa by applying the Psp transition slope based on Fei et al. (2004). Thus, the present transition pressure completely agrees with the D660 depth. The reason for the lower transition pressures by the previous studies is pressure drop during heating. Although the transition completes at the beginning of target temperature, pressure significantly drops during or even before accumulating a diffraction

In-situ high-pressure powder X-ray diffraction study of α-zirconium phosphate.

PubMed

Readman, Jennifer E; Lennie, Alistair; Hriljac, Joseph A

2014-06-01

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied using in-situ high-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus, K0 = 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr-O-P.

High-resistive layers obtained through periodic growth and in situ annealing of InGaN by metalorganic chemical vapor deposition

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

Zhang, Shuo; Ma, Ping, E-mail: maping@semi.ac.cn; Liu, Boting

2016-06-15

High-resistive layers were obtained by periodic growth and in situ annealing of InGaN. The effect of the annealing temperature of InGaN on the indium content and the material sheet resistive was investigated. The indium content decreased as the increase of in situ annealing temperature. Additionally, the material sheet resistance increased with the increase of the in situ annealing temperature for the annealed samples and reached 2 × 10{sup 10}Ω/sq in the light and 2 × 10{sup 11}Ω/sq in the dark when the in situ annealing temperature reached 970{sup ∘}C. The acquirement of high-resistive layers is attributed to the generation ofmore » indium vacancy-related defects. Introducing indium vacancy-related defects to compensate background carriers can be an effective method to grow high-resistance material.« less

Short-period cyclic loading system for in situ X-ray observation of anelastic properties at high pressure.

PubMed

Yoshino, Takashi; Yamazaki, Daisuke; Tange, Yoshinori; Higo, Yuji

2016-10-01

To determine the anelastic properties of materials of the Earth's interior, a short-period cyclic loading system was installed for in situ X-ray radiographic observation under high pressure to the multi-anvil deformation DIA press at the bending magnet beam line BL04B1 at SPring-8. The hydraulic system equipped with a piston controlled by a solenoid was designed so as to enable producing smooth sinusoidal stress in a wide range of oscillation period from 0.2 to 100 s and generating variable amplitudes. Time resolved X-ray radiography imaging of the sample and reference material provides their strain as a function of time during cyclic loading. A synchrotron X-ray radiation source allows us to resolve their strain variation with time even at the short period (<1 s). The minimum resolved strain is as small as 10 -4 , and the shortest oscillation period to detect small strain is 0.5 s. Preliminary experimental results exhibited that the new system can resolve attenuation factor Q -1 at upper mantle conditions. These results are in quantitative agreement with previously reported data obtained at lower pressures.

Apparatus for in-situ calibration of instruments that measure fluid depth

DOEpatents

Campbell, M.D.

1994-01-11

The present invention provides a method and apparatus for in-situ calibration of distance measuring equipment. The method comprises obtaining a first distance measurement in a first location, then obtaining at least one other distance measurement in at least one other location of a precisely known distance from the first location, and calculating a calibration constant. The method is applied specifically to calculating a calibration constant for obtaining fluid level and embodied in an apparatus using a pressure transducer and a spacer of precisely known length. The calibration constant is used to calculate the depth of a fluid from subsequent single pressure measurements at any submerged position. 8 figures.

Apparatus for in-situ calibration of instruments that measure fluid depth

DOEpatents

Campbell, Melvin D.

1994-01-01

The present invention provides a method and apparatus for in-situ calibration of distance measuring equipment. The method comprises obtaining a first distance measurement in a first location, then obtaining at least one other distance measurement in at least one other location of a precisely known distance from the first location, and calculating a calibration constant. The method is applied specifically to calculating a calibration constant for obtaining fluid level and embodied in an apparatus using a pressure transducer and a spacer of precisely known length. The calibration constant is used to calculate the depth of a fluid from subsequent single pressure measurements at any submerged position.

In situ stress and pore pressure in the Kumano Forearc Basin, offshore SW Honshu from downhole measurements during riser drilling

NASA Astrophysics Data System (ADS)

Saffer, D. M.; Flemings, P. B.; Boutt, D.; Doan, M.-L.; Ito, T.; McNeill, L.; Byrne, T.; Conin, M.; Lin, W.; Kano, Y.; Araki, E.; Eguchi, N.; Toczko, S.

2013-05-01

situ stress and pore pressure are key parameters governing rock deformation, yet direct measurements of these quantities are rare. During Integrated Ocean Drilling Program (IODP) Expedition #319, we drilled through a forearc basin at the Nankai subduction zone and into the underlying accretionary prism. We used the Modular Formation Dynamics Tester tool (MDT) for the first time in IODP to measure in situ minimum stress, pore pressure, and permeability at 11 depths between 729.9 and 1533.9 mbsf. Leak-off testing at 708.6 mbsf conducted as part of drilling operations provided a second measurement of minimum stress. The MDT campaign included nine single-probe (SP) tests to measure permeability and in situ pore pressure and two dual-packer (DP) tests to measure minimum principal stress. Permeabilities defined from the SP tests range from 6.53 × 10-17 to 4.23 × 10-14 m2. Pore fluid pressures are near hydrostatic throughout the section despite rapid sedimentation. This is consistent with the measured hydraulic diffusivity of the sediments and suggests that the forearc basin should not trap overpressures within the upper plate of the subduction zone. Minimum principal stresses are consistently lower than the vertical stress. We estimate the maximum horizontal stress from wellbore failures at the leak-off test and shallow MDT DP test depths. The results indicate a normal or strike-slip stress regime, consistent with the observation of abundant active normal faults in the seaward-most part of the basin, and a general decrease in fault activity in the vicinity of Site C0009.

In situ study of maize starch gelatinization under ultra-high hydrostatic pressure using X-ray diffraction.

PubMed

Yang, Zhi; Gu, Qinfen; Hemar, Yacine

2013-08-14

The gelatinization of waxy (very low amylose) and high-amylose maize starches by ultra-high hydrostatic pressure (up to 6 GPa) was investigated in situ using synchrotron X-ray powder diffraction on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio, were pressurized and measured at room temperature. X-ray diffraction pattern showed that at 2.7 GPa waxy starch, which displayed A-type XRD pattern at atmospheric pressure, exhibited a faint B-type-like pattern. The B-type crystalline structures of high-amylose starch were not affected even when 1.5 GPa pressure was applied. However, both waxy and high-amylose maize starches can be fully gelatinized at 5.9 GPa and 5.1 GPa, respectively. In the case of waxy maize starch, upon release of pressure (to atmospheric pressure) crystalline structure appeared as a result of amylopectin aggregation. Copyright © 2013 Elsevier Ltd. All rights reserved.

Examination of the Atomic Pair Distribution Function (PDF) of SiC Nanocrystals by In-situ High Pressure Diffraction

NASA Technical Reports Server (NTRS)

Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Zhao, Y.; Palosz, B.; Palosz, W.

2003-01-01

Key properties of nanocrystals are determined by their real atomic structure, therefore a reasonable understanding and meaningful interpretation of their properties requires a realistic model of the structure. In this paper we present an evidence of a complex response of the lattice distances to external pressure indicating a presence of a complex structure of Sic nanopowders. The experiments were performed on nanocrystalline Sic subjected to hydrostatic or isostatic pressure using synchrotron and neutron powder diffraction. Elastic properties of the samples were examined based on X-ray diffraction data using a Diamond Anvil Cell (DAC) in HASYLAB at DESY. The dependence'of the lattice parameters and of the Bragg reflections width with pressure exhibits a ha1 nature of the properties (compressibilities) of the powders and indicates a complex structure of the grains. We interpreted tws behaviour as originating from different elastic properties of the grain interior and surface. Analysis of the dependence of individual interatomic distances on pressure was based on in-situ neutron diffraction measurements done with HbD diffractometer at LANSCE in Los Alamos National Laboratory with the Paris-Edinburgh cell under pressures up to 8 GPa (Qmax = 26/A). Interatomic distances were obtained by PDF analysis using the PDFgetN program. We have found that the interatomic distances undergo a complex, non-monotonic changes. Even under substantial pressures a considerable relaxation of the lattice may take place: some interatomic distances increase with an increase in pressure. We relate this phenomenon to: (1), changes of the microstructure of the densified material, in particular breaking of its fractal chain structure and, (2), its complex structure resembling that of a material composed of two phases, each with its distinct elastic properties.

Investigation of the Surface Stress in SiC and Diamond Nanocrystals by In-situ High Pressure Powder Diffraction Technique

NASA Technical Reports Server (NTRS)

Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Zhao, Y.; Palosz, W.

2003-01-01

The real atomic structure of nanocrystals determines key properties of the materials. For such materials the serious experimental problem lies in obtaining sufficiently accurate measurements of the structural parameters of the crystals, since very small crystals constitute rather a two-phase than a uniform crystallographic phase system. As a result, elastic properties of nanograins may be expected to reflect a dual nature of their structure, with a corresponding set of different elastic property parameters. We studied those properties by in-situ high-pressure powder diffraction technique. For nanocrystalline, even one-phase materials such measurements are particularly difficult to make since determination of the lattice parameters of very small crystals presents a challenge due to inherent limitations of standard elaboration of powder diffractograms. In this investigation we used our methodology of the structural analysis, the 'apparent lattice parameter' (alp) concept. The methodology allowed us to avoid the traps (if applied to nanocrystals) of standard powder diffraction evaluation techniques. The experiments were performed for nanocrystalline Sic and GaN powders using synchrotron sources. We applied both hydrostatic and isostatic pressures in the range of up to 40 GPa. Elastic properties of the samples were examined based on the measurements of a change of the lattice parameters with pressure. The results show a dual nature of the mechanical properties (compressibilities) of the materials, indicating a complex, core-shell structure of the grains.

Highly conductive and transparent thin ZnO films prepared in situ in a low pressure system

NASA Astrophysics Data System (ADS)

Ataev, B. M.; Bagamadova, A. M.; Mamedov, V. V.; Omaev, A. K.; Rabadanov, M. R.

1999-03-01

Sucessful preparation of ZnO : M epitaxial thin films (ETF) in situ doped with donor impurity M=Ga, Sn by chemical vapor despsition in a low-pressure system is reported. Highly conductive (up to 10 -4 Ω cm) and transparent ( T>85%) ZnO : M ETF have been successfully produced on single crystal (1012) sapphire substrates. Electrical properties of the films as well as their excition luminescence were studied.

In situ pore-pressure evolution during dynamic CPT measurements in soft sediments of the western Baltic Sea

NASA Astrophysics Data System (ADS)

Seifert, Annedore; Stegmann, Sylvia; Mörz, Tobias; Lange, Matthias; Wever, Thomas; Kopf, Achim

2008-08-01

We present in situ strength and pore-pressure measurements from 57 dynamic cone penetration tests in sediments of Mecklenburg ( n = 51), Eckernförde ( n = 2) and Gelting ( n = 4) bays, western Baltic Sea, characterised by thick mud layers and partially free microbial gas resulting from the degradation of organic material. In Mecklenburg and Eckernförde bays, sediment sampling by nine gravity cores served sedimentological characterisation, analyses of geotechnical properties, and laboratory shear tests. At selected localities, high-resolution echo-sounder profiles were acquired. Our aim was to deploy a dynamic cone penetrometer (CPT) to infer sediment shear strength and cohesion of the sea bottom as a function of fluid saturation. The results show very variable changes in pore pressure and sediment strength during the CPT deployments. The majority of the CPT measurements ( n = 54) show initially negative pore-pressure values during penetration, and a delayed response towards positive pressures thereafter. This so-called type B pore-pressure signal was recorded in all three bays, and is typically found in soft muds with high water contents and undrained shear strengths of 1.6-6.4 kPa. The type B signal is further affected by displacement of sediment and fluid upon penetration of the lance, skin effects during dynamic profiling, enhanced consolidation and strength of individual horizons, the presence of free gas, and a dilatory response of the sediment. In Mecklenburg Bay, the remaining small number of CPT measurements ( n = 3) show a well-defined peak in both pore pressure and cone resistance during penetration, i.e. an initial marked increase which is followed by exponential pore-pressure decay during dissipation. This so-called type A pore-pressure signal is associated with normally consolidated mud, with indurated clay layers showing significantly higher undrained shear strength (up to 19 kPa). In Eckernförde and Gelting bays pore-pressure response type B is

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritical conditions

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

Diefenbacher, Jason; McKelvy, Michael; Chizmeshya, Andrew V.G.

2005-01-01

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 deg. C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full opticalmore » accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritial conditions

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

Diefenbacher, J.; McKelvy, M.; Chizemeshya, A.V.

2010-07-13

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibilitymore » and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Reliability and Accuracy of Static Parameters Obtained From Ink and Pressure Platform Footprints.

PubMed

Zuil-Escobar, Juan Carlos; Martínez-Cepa, Carmen Belén; Martín-Urrialde, Jose Antonio; Gómez-Conesa, Antonia

2016-09-01

The purpose of this study was to evaluate the accuracy and the intrarater reliability of arch angle (AA), Staheli Index (SI), and Chippaux-Smirak Index (CSI) obtained from ink and pressure platform footprints. We obtained AA, SI, and CSI measurements from ink pedigraph footprints and pressure platform footprints in 40 healthy participants (aged 25.65 ± 5.187 years). Intrarater reliability was calculated for all parameters obtained using the 2 methods. Standard error of measurement and minimal detectable change were also calculated. A repeated-measure analysis of variance was used to identify differences between ink and pressure platform footprints. Intraclass correlation coefficient and Bland and Altman plots were used to assess similar parameters obtained using different methods. Intrarater reliability was >0.9 for all parameters and was slightly higher for the ink footprints. No statistical difference was reported in repeated-measure analysis of variance for any of the parameters. Intraclass correlation coefficient values from AA, SI, and CSI that were obtained using ink footprints and pressure platform footprints were excellent, ranging from 0.797 to 0.829. However, pressure platform overestimated AA and underestimated SI and CSI. Our study revealed that AA, SI, and CSI were similar regardless of whether the ink or pressure platform method was used. In addition, the parameters indicated high intrarater reliability and were reproducible. Copyright © 2016. Published by Elsevier Inc.

The lunar semidiurnal air pressure tide in in-situ data and ECMWF reanalyses

NASA Astrophysics Data System (ADS)

Schindelegger, Michael; Dobslaw, Henryk

2016-04-01

A gridded empirical model of the lunar semidiurnal air pressure tide L2 is deduced through multiquadric interpolation of more than 2000 globally distributed tidal estimates from land barometers and moored buoys. The resulting climatology serves as an independent standard to validate the barometric L2 oscillations that are present in ECMWF's (European Centre for Medium-Range Weather Forecasts) global atmospheric reanalyses despite the omission of gravitational forcing mechanisms in the involved forecast routines. Inconsistencies between numerical and empirical L2 solutions are found to be small even though the reanalysis models typically underestimate equatorial peak pressures by 10-20% and produce slightly deficient tidal phases in latitudes south of 30°N. Through using a time-invariant reference surface over both land and water and assimilating marine pressure data without accounting for vertical sensor movements due to the M2 ocean tide, ECMWF-based tidal solutions are also prone to strong local artifacts. Additionally, the dependency of the lunar tidal oscillation in atmospheric analysis systems on the meteorological input data is demonstrated based on a recent ECMWF twentieth-century reanalysis (ERA-20C) which draws its all of its observational constraints from in-situ registrations of pressure and surface winds. The L2 signature prior to 1950 is particularly indicative of distinct observing system changes, such as the paucity of marine data during both World Wars or the opening of the Panama Canal in 1914 and the associated adjustment of commercial shipping routes.

Bridging a possible gap of GRACE observations in the Arctic Ocean using existing GRACE data and in situ bottom pressure sensors

NASA Astrophysics Data System (ADS)

Peralta Ferriz, C.; Morison, J.

2014-12-01

Since 2003, the Gravity Recovery and Climate Experiment (GRACE) satellite system has provided the means of investigating month-to-month to inter-annual variability of, among many other things, Arctic Ocean circulation over the entire Arctic Basin. Such a comprehensive picture could not have been achieved with the limited in situ pressure observations available. Results from the first 10 years of ocean bottom pressure measurements from GRACE in the Arctic Ocean reveal distinct patterns of ocean variability that are strongly associated with changes in large-scale atmospheric circulation (Peralta-Ferriz et al., 2014): the leading mode of variability being a wintertime basin-coherent mass change driven by winds in the Nordic Seas; the second mode of variability corresponding to a mass signal coherent along the Siberian shelves, and driven by the Arctic Oscillation; and the third mode being a see-saw between western and eastern Arctic shelves, also driven by the large-scale wind patterns. In order to understand Arctic Ocean changes, it is fundamental to continue to track ocean bottom pressure. Our concern is what to do if the present GRACE system, which is already well beyond its design lifetime, should fail before its follow-on is launched, currently estimated to be in 2017. In this work, we regress time series of pressure from the existing and potential Arctic Ocean bottom pressure recorder locations against the fundamental modes of bottom pressure variation. Our aim is to determine the optimum combination of in situ measurements to represent the broader scale variability now observed by GRACE. With this understanding, we can be better prepared to use in situ observations to at least partially cover a possible gap in GRACE coverage. Reference:Peralta-Ferriz, Cecilia, James H. Morison, John M. Wallace, Jennifer A. Bonin, Jinlun Zhang, 2014: Arctic Ocean Circulation Patterns Revealed by GRACE. J. Climate, 27, 1445-1468. doi: http://dx.doi.org/10.1175/JCLI-D-13-00013.1

Semiconductor Clathrates: In Situ Studies of Their High Pressure, Variable Temperature and Synthesis Behavior

NASA Astrophysics Data System (ADS)

Machon, D.; McMillan, P. F.; San-Miguel, A.; Barnes, P.; Hutchins, P. T.

In situ studies have provided valuable new information on the synthesis mechanisms, low temperature properties and high pressure behavior of semiconductor clathrates. Here we review work using synchrotron and laboratory X-ray diffraction and Raman scattering used to study mainly Si-based clathrates under a variety of conditions. During synthesis of the Type I clathrate Na8Si46 by metastable thermal decomposition from NaSi in vacuum, we observe an unusual quasi-epitaxial process where the clathrate structure appears to nucleate and grow directly from the Na-deficient Zintl phase surface. Low temperature X-ray studies of the guest-free Type II clathrate framework Si136 reveal a region of negative thermal expansion behavior as predicted theoretically and analogous to that observed for diamond-structured Si. High pressure studies of Si136 lead to metastable production of the β-Sn structured Si-II phase as well as perhaps other metastable crystalline materials. High pressure investigations of Type I clathrates show evidence for a new class of apparently isostructural densification transformations followed by amorphization in certain cases.

Structural Transitions in Nanosized Zn0.97Al0.03O Powders under High Pressure Analyzed by in Situ Angle-Dispersive X-ray Diffraction

PubMed Central

Lin, Chih-Ming; Liu, Hsin-Tzu; Zhong, Shi-Yao; Hsu, Chia-Hung; Chiu, Yi-Te; Tai, Ming-Fong; Juang, Jenh-Yih; Chuang, Yu-Chun; Liao, Yen-Fa

2016-01-01

Nanosized aluminum-doped zinc oxide Zn1−xAlxO (AZO) powders (AZO-NPs) with x = 0.01, 0.03, 0.06, 0.09 and 0.11 were synthesized by chemical precipitation method. The thermogravimetric analysis (TGA) indicated that the precursors were converted to oxides from hydroxides near 250 °C, which were then heated to 500 °C for subsequent thermal processes to obtain preliminary powders. The obtained preliminary powders were then calcined at 500 °C for three hours. The structure and morphology of the products were measured and characterized by angle-dispersive X-ray diffraction (ADXRD) and scanning electron microscopy (SEM). ADXRD results showed that AZO-NPs with Al content less than 11% exhibited würtzite zinc oxide structure and there was no other impurity phase in the AZO-NPs, suggesting substitutional doping of Al on Zn sites. The Zn0.97Al0.03O powders (A3ZO-NPs) with grain size of about 21.4 nm were used for high-pressure measurements. The in situ ADXRD measurements revealed that, for loading run, the pressure-induced würtzite (B4)-to-rocksalt (B1) structural phase transition began at 9.0(1) GPa. Compared to the predicted phase-transition pressure of ~12.7 GPa for pristine ZnO nanocrystals of similar grain size (~21.4 nm), the transition pressure for the present A3ZO-NPs exhibited a reduction of ~3.7 GPa. The significant reduction in phase-transition pressure is attributed to the effects of highly selective site occupation, namely Zn2+ and Al3+, were mainly found in tetrahedral and octahedral sites, respectively. PMID:28773683

[Evaluation of soy bean proteins obtained by pressure].

PubMed

Bau, H M; Poullain, B; Debry, G

1978-01-01

Besides the processes of extrusion and protein fiber spinning, analogous utilization research with a range of protein sources is continuing at an accelerated pace. However, the pressure forming process, an attractive process for producing protein foods, has not received the attention as it merits. The fabrication techniques contribute the advantages of nutritional value, economic and simplicity in manufacture; it can be extend to utilize in the development of useful textured vegetable protein foods. Here, we present a pressure forming process for producing protein foods with soybean grains. In this paper, we evaluated the composition, and the yield of the products obtained by this process; the trypsin inhibitor and enzymatic proteolyse of the products were also studied. The product obtained contents soluble and insoluble proteins of soybean, 45 p. 100 of protein (N x 6,25), 20-25 p. 100 of carbohydrates of which the fibers are included; moreover it contents 6-7 p. 100 of ash and 20-22 p. 100 of fat. It does not content any starch, the oligosaccharides and antinutritional factors were almost eliminated. This product presents in acceptable textural form resembling traditional animal protein foodstuffs; its fonctional and nutritional properties can meet different utilizations in foodstuffs such as dietetic products and protein complements.

Capillary pressure curves for low permeability chalk obtained by NMR imaging of core saturation profiles

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

Norgaard, J.V.; Olsen, D.; Springer, N.

1995-12-31

A new technique for obtaining water-oil capillary pressure curves, based on NMR imaging of the saturation distribution in flooded cores is presented. In this technique, a steady state fluid saturation profile is developed by flooding the core at a constant flow rate. At the steady state situation where the saturation distribution no longer changes, the local pressure difference between the wetting and non-wetting phases represents the capillary pressure. The saturation profile is measured using an NMR technique and for a drainage case, the pressure in the non-wetting phase is calculated numerically. The paper presents the NMR technique and the proceduremore » for calculating the pressure distribution in the sample. Inhomogeneous samples produce irregular saturation profiles, which may be interpreted in terms of variation in permeability, porosity, and capillary pressure. Capillary pressure curves for North Sea chalk obtained by the new technique show good agreement with capillary pressure curves obtained by traditional techniques.« less

A novel APPI-MS setup for in situ degradation product studies of atmospherically relevant compounds: capillary atmospheric pressure photo ionization (cAPPI).

PubMed

Kersten, Hendrik; Derpmann, Valerie; Barnes, Ian; Brockmann, Klaus J; O'Brien, Rob; Benter, Thorsten

2011-11-01

We report on the development of a novel atmospheric pressure photoionization setup and its applicability for in situ degradation product studies of atmospherically relevant compounds. A custom miniature spark discharge lamp was embedded into an ion transfer capillary, which separates the atmospheric pressure from the low pressure region in the first differential pumping stage of a conventional atmospheric pressure ionization mass spectrometer. The lamp operates with a continuous argon flow and produces intense light emissions in the VUV. The custom lamp is operated windowless and efficiently illuminates the sample flow through the transfer capillary on an area smaller than 1 mm(2). Limits of detection in the lower ppbV range, a temporal resolution of milliseconds in the positive as well as the quasi simultaneously operating negative ion mode, and a significant reduction of ion transformation processes render this system applicable to real time studies of rapidly changing chemical systems. The method termed capillary atmospheric pressure photo ionization (cAPPI) is characterized with respect to the lamp emission properties as a function of the operating conditions, temporal response, and its applicability for in situ degradation product studies of atmospherically relevant compounds, respectively.

Description of a Pressure Measurement Technique for Obtaining Surface Static Pressures of a Radial Turbine

NASA Technical Reports Server (NTRS)

Dicicco, L. Danielle; Nowlin, Brent C.; Tirres, Lizet

1992-01-01

The aerodynamic performance of a solid uncooled version of a cooled radial turbine was evaluated in the Small Engine Components Test Facility Turbine rig at the NASA Lewis Research Center. Specifically, an experiment was conducted to rotor surface static pressures. This was the first time surface static pressures had been measured on a radial turbine at NASA Lewis. These pressures were measured by a modified Rotating Data Package (RDP), a standard product manufactured by Scanivalve, Inc. Described here are the RDP, and the modifications that were made, as well as the checkout, installation, and testing procedures. The data presented are compared to analytical results obtained from NASA's MERIDL TSONIC BLAYER (MTSB) code.

Description of a pressure measurement technique for obtaining surface static pressures of a radial turbine

NASA Technical Reports Server (NTRS)

Dicicco, L. D.; Nowlin, Brent C.; Tirres, Lizet

1992-01-01

The aerodynamic performance of a solid uncooled version of a cooled radial turbine was evaluated in the Small Engine Components Test Facility Turbine rig at the NASA Lewis Research Center. Specifically, an experiment was conducted to rotor surface static pressures. This was the first time surface static pressures had been measured on a radial turbine at NASA Lewis. These pressures were measured by a modified Rotating Data Package (RDP), a standard product manufactured by Scanivalve, Inc. Described here are the RDP, and the modifications that were made, as well as the checkout, installation, and testing procedures. The data presented are compared to analytical results obtained from NASA's MERIDL TSONIC BLAYER (MTSB) code.

TDLAS-based sensors for in situ measurement of syngas composition in a pressurized, oxygen-blown, entrained flow coal gasifier

NASA Astrophysics Data System (ADS)

Sur, Ritobrata; Sun, Kai; Jeffries, Jay B.; Hanson, Ronald K.; Pummill, Randy J.; Waind, Travis; Wagner, David R.; Whitty, Kevin J.

2014-07-01

Tunable diode laser absorption spectroscopy based in situ sensors for CO (2.33 μm), CO2 (2.02 μm), CH4 (2.29 μm) and H2O (1.35 μm) were deployed in a pilot-scale (1 ton/day), high-pressure (up to 18 atm), entrained flow, oxygen-blown, slagging coal gasifier at the University of Utah. Measurements of species mole fraction with 3-s time resolution were taken at the pre- and post-filtration stages of the gasifier synthesis gas (called here syngas) output flow. Although particulate scattering makes pre-filter measurements more difficult, this location avoids the time delay of flow through the filtration devices. With the measured species and known N2 concentrations, the H2 content was obtained via balance. The lower heating value and the Wobbe index of the gas mixture were estimated using the measured gas composition. The sensors demonstrated here show promise for monitoring and control of the gasification process.

In situ Raman and X-ray diffraction studies on the high pressure and temperature stability of methane hydrate up to 55 GPa.

PubMed

Kadobayashi, Hirokazu; Hirai, Hisako; Ohfuji, Hiroaki; Ohtake, Michika; Yamamoto, Yoshitaka

2018-04-28

High-temperature and high-pressure experiments were performed under 2-55 GPa and 298-653 K using in situ Raman spectroscopy and X-ray diffraction combined with externally heated diamond anvil cells to investigate the stability of methane hydrate. Prior to in situ experiments, the typical C-H vibration modes of methane hydrate and their pressure dependence were measured at room temperature using Raman spectroscopy to make a clear discrimination between methane hydrate and solid methane which forms through the decomposition of methane hydrate at high temperature. The sequential in situ Raman spectroscopy and X-ray diffraction revealed that methane hydrate survives up to 633 K and 40.3 GPa and then decomposes into solid methane and ice VII above the conditions. The decomposition curve of methane hydrate estimated by the present experiments is >200 K lower than the melting curves of solid methane and ice VII, and moderately increases with increasing pressure. Our result suggests that although methane hydrate may be an important candidate for major constituents of cool exoplanets and other icy bodies, it is unlikely to be present in the ice mantle of Neptune and Uranus, where the temperature is expected to be far beyond the decomposition temperatures.

In situ Raman and X-ray diffraction studies on the high pressure and temperature stability of methane hydrate up to 55 GPa

NASA Astrophysics Data System (ADS)

Kadobayashi, Hirokazu; Hirai, Hisako; Ohfuji, Hiroaki; Ohtake, Michika; Yamamoto, Yoshitaka

2018-04-01

High-temperature and high-pressure experiments were performed under 2-55 GPa and 298-653 K using in situ Raman spectroscopy and X-ray diffraction combined with externally heated diamond anvil cells to investigate the stability of methane hydrate. Prior to in situ experiments, the typical C-H vibration modes of methane hydrate and their pressure dependence were measured at room temperature using Raman spectroscopy to make a clear discrimination between methane hydrate and solid methane which forms through the decomposition of methane hydrate at high temperature. The sequential in situ Raman spectroscopy and X-ray diffraction revealed that methane hydrate survives up to 633 K and 40.3 GPa and then decomposes into solid methane and ice VII above the conditions. The decomposition curve of methane hydrate estimated by the present experiments is >200 K lower than the melting curves of solid methane and ice VII, and moderately increases with increasing pressure. Our result suggests that although methane hydrate may be an important candidate for major constituents of cool exoplanets and other icy bodies, it is unlikely to be present in the ice mantle of Neptune and Uranus, where the temperature is expected to be far beyond the decomposition temperatures.

In situ hydrostatic pressure induced improvement of critical current density and suppression of magnetic relaxation in Y(Dy0.5)Ba2Cu3O7‑δ coated conductors

NASA Astrophysics Data System (ADS)

Sang, Lina; Gutiérrez, Joffre; Cai, Chuanbing; Dou, Shixue; Wang, Xiaolin

2018-07-01

We report on the effect of in situ hydrostatic pressure on the enhancement of the in-magnetic-field critical current density parallel to the crystallographic c-axis and vortex pinning in epitaxial Y(Dy0.5)Ba2Cu3O7‑δ coated conductors prepared by metal organic deposition. Our results show that in situ hydrostatic pressure greatly enhances the critical current density at high fields and high temperatures. At 80 K and 5 T we observe a ten-fold increase in the critical current density under the pressure of 1.2 GPa, and the irreversibility line is shifted to higher fields without changing the critical temperature. The normalized magnetic relaxation rate shows that vortex creep rates are strongly suppressed due to applied pressure, and the pinning energy is significantly increased based on the collective creep theory. After releasing the pressure, we recover the original superconducting properties. Therefore, we speculate that the in situ hydrostatic pressure exerted on the coated conductor enhances the pinning of existing extended defects. This is totally different from what has been observed in REBa2Cu3O7‑δ melt-textured crystals, where the effect of pressure generates point-like defects.

Measuring in-vivo and in-situ ex-vivo the 3D deformation of the lamina cribrosa microstructure under elevated intraocular pressure

NASA Astrophysics Data System (ADS)

Wei, Junchao; Yang, Bin; Voorhees, Andrew P.; Tran, Huong; Brazile, Bryn; Wang, Bo; Schuman, Joel; Smith, Matthew A.; Wollstein, Gadi; Sigal, Ian A.

2018-02-01

Elevated intraocular pressure (IOP) deforms the lamina cribrosa (LC), a structure within the optic nerve head (ONH) in the back of the eye. Evidence suggests that these deformations trigger events that eventually cause irreversible blindness, and have therefore been studied in-vivo using optical coherence tomography (OCT), and ex-vivo using OCT and a diversity of techniques. To the best of our knowledge, there have been no in-situ ex-vivo studies of LC mechanics. Our goal was two-fold: to introduce a technique for measuring 3D LC deformations from OCT, and to determine whether deformations of the LC induced by elevated IOP differ between in-vivo and in-situ ex-vivo conditions. A healthy adult rhesus macaque monkey was anesthetized and IOP was controlled by inserting a 27- gauge needle into the anterior chamber of the eye. Spectral domain OCT was used to obtain volumetric scans of the ONH at normal and elevated IOPs. To improve the visibility of the LC microstructure the scans were first processed using a novel denoising technique. Zero-normalized cross-correlation was used to find paired corresponding locations between images. For each location pair, the components of the 3D strain tensor were determined using non-rigid image registration. A mild IOP elevation from 10 to 15mmHg caused LC effective strains as large as 3%, and about 50% larger in-vivo than in-situ ex-vivo. The deformations were highly heterogeneous, with substantial 3D components, suggesting that accurate measurement of LC microstructure deformation requires high-resolution volumes. This technique will help improve understanding of LC biomechanics and how IOP contributes to glaucoma.

Hydraulic High Pressure Valve Controller Using the In-Situ Pressure Difference

NASA Technical Reports Server (NTRS)

Badescu, Mircea (Inventor); Bar-Cohen, Yoseph (Inventor); Hall, Jeffery L. (Inventor); Sherrit, Stewart (Inventor); Bao, Xiaoqi (Inventor)

2016-01-01

A hydraulic valve controller that uses an existing pressure differential as some or all of the power source for valve operation. In a high pressure environment, such as downhole in an oil or gas well, the pressure differential between the inside of a pipe and the outside of the pipe may be adequately large to drive a linear slide valve. The valve is operated hydraulically by a piston in a bore. When a higher pressure is applied to one end of the bore and a lower pressure to the other end, the piston moves in response to the pressure differential and drives a valve attached to it. If the pressure differential is too small to drive the piston at a sufficiently high speed, a pump is provided to generate a larger pressure differential to be applied. The apparatus is conveniently constructed using multiport valves, which can be rotary valves.

Different seismic signatures of fractures slip and their correlations with fluid pressures in in-situ rupture experiments

NASA Astrophysics Data System (ADS)

Derode, B.; Cappa, F.; Guglielmi, Y.

2012-04-01

The recent observations of non-volcanic tremors (NVT), slow-slip events (SSE), low- (LFE) and very-low (VLF) frequency earthquakes on seismogenic faults reveal that unexpected, large, non-linear transient deformations occur during the interseismic loading of the earthquake cycle. Such phenomena modify stress to the adjacent locked zones bringing them closer to failure. Recent studies indicated various driving factors such as high-fluid pressures and frictional processes. Here we focus on the role of fluids in the different seismic signatures observed in in-situ fractures slip experiments. Experiments were conducted in critically stressed fractures zone at 250 m-depth within the LSBB underground laboratory (south of France). This experiment seeks to explore the field measurements of temporal variations in fluid and stress through continuous monitoring of seismic waves, fluid pressures and mechanical deformations between boreholes and the ground surface. The fluid pressure was increased step-by-step in a fracture isolated between packers until a maximum value of 35 bars; a pressure analog to ones known to trigger earthquakes at crustal depths. We observed in the seismic signals: (1) Tremor-like signatures, (2) Low Frequency signatures, and (3) sudden and short ruptures like micro-earthquakes. By analogy, we suggest that fluid pressures may trigger these different seismic signatures in active faults.

Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts

NASA Astrophysics Data System (ADS)

Zhao, Z.; Diemant, T.; Häring, T.; Rauscher, H.; Behm, R. J.

2005-12-01

We describe the design and performance of a high-pressure reaction cell for simultaneous kinetic and in situ infrared reflection (IR) spectroscopic measurements on model catalysts at elevated pressures, between 10-3 and 103mbars, which can be operated both as batch reactor and as flow reactor with defined gas flow. The cell is attached to an ultrahigh-vacuum (UHV) system, which is used for sample preparation and also contains facilities for sample characterization. Specific for this design is the combination of a small cell volume, which allows kinetic measurements with high sensitivity under batch or continuous flow conditions, the complete isolation of the cell from the UHV part during UHV measurements, continuous temperature control during both UHV and high-pressure operation, and rapid transfer between UHV and high-pressure stage. Gas dosing is performed by a designed gas-handling system, which allows operation as flow reactor with calibrated gas flows at adjustable pressures. To study the kinetics of reactions on the model catalysts, a quadrupole mass spectrometer is connected to the high-pressure cell. IR measurements are possible in situ by polarization-modulation infrared reflection-absorption spectroscopy, which also allows measurements at elevated pressures. The performance of the setup is demonstrated by test measurements on the kinetics for CO oxidation and the CO adsorption on a Au /TiO2/Ru(0001) model catalyst film at 1-50 mbar total pressure.

A High Temperature Capacitive Pressure Sensor Based on Alumina Ceramic for in Situ Measurement at 600 °C

PubMed Central

Tan, Qiulin; Li, Chen; Xiong, Jijun; Jia, Pinggang; Zhang, Wendong; Liu, Jun; Xue, Chenyang; Hong, Yingping; Ren, Zhong; Luo, Tao

2014-01-01

In response to the growing demand for in situ measurement of pressure in high-temperature environments, a high temperature capacitive pressure sensor is presented in this paper. A high-temperature ceramic material-alumina is used for the fabrication of the sensor, and the prototype sensor consists of an inductance, a variable capacitance, and a sealed cavity integrated in the alumina ceramic substrate using a thick-film integrated technology. The experimental results show that the proposed sensor has stability at 850 °C for more than 20 min. The characterization in high-temperature and pressure environments successfully demonstrated sensing capabilities for pressure from 1 to 5 bar up to 600 °C, limited by the sensor test setup. At 600 °C, the sensor achieves a linear characteristic response, and the repeatability error, hysteresis error and zero-point drift of the sensor are 8.3%, 5.05% and 1%, respectively. PMID:24487624

In situ Raman and synchrotron X-ray diffraction study on crystallization of Choline chloride/Urea deep eutectic solvent under high pressure

NASA Astrophysics Data System (ADS)

Yuan, Chaosheng; Chu, Kunkun; Li, Haining; Su, Lei; Yang, Kun; Wang, Yongqiang; Li, Xiaodong

2016-09-01

Pressure-induced crystallization of Choline chloride/Urea (ChCl/Urea) deep eutectic solvent (DES) has been investigated by in-situ Raman spectroscopy and synchrotron X-ray diffraction. The results indicated that high pressure crystals appeared at around 2.6 GPa, and the crystalline structure was different from that formed at ambient pressure. Upon increasing the pressure, the Nsbnd H stretching modes of Urea underwent dramatic change after liquid-solid transition. It appears that high pressures may enhance the hydrogen bonds formed between ChCl and Urea. P versus T phase diagram of ChCl/Urea DES was constructed, and the crystallization mechanism of ChCl/Urea DES was discussed in view of hydrogen bonds.

In situ studies of velocity in fractured crystalline rocks.

USGS Publications Warehouse

Moos, D.; Zoback, M.D.

1983-01-01

A study of the effects of macroscopic fractures on P and S wave velocities has been conducted in four wells drilled in granitic rock to depths between 0.6 and 1.2km. The effect of macroscopic fractures is to decrease both Vp and Vs and increase Vp/Vs. In wells with a relatively low density of macroscopic fractures, the in situ velocity is similar to that of saturated core samples under confining pressure in the laboratory, and there is a clear correlation between zones with macroscopic fractures and anomalously low velocities. In wells with numerous macroscopic fractures, the in situ velocity is lower than that of intact samples under pressure, and there is a correlation between the rate at which in situ velocity increases with depth and the rate at which the velocity of laboratory samples increases with pressure. Differences in in situ P wave velocity between wells cannot be explained solely by differences in the degree of macroscopic fracturing, thus emphasizing the importance of composition and microcracks on velocity.-from Authors

Strategies for obtaining long constant-pressure test times in shock tubes

DOE PAGES

Campbell, Matthew Frederick; Parise, T.; Tulgestke, A. M.; ...

2015-09-22

Several techniques have been developed for obtaining long, constant-pressure test times in reflected shock wave experiments in a shock tube, including the use of driver inserts, driver gas tailoring, helium gas diaphragm interfaces, driver extensions, and staged driver gas filling. Here, we detail these techniques, including discussion on the most recent strategy, staged driver gas filling. Experiments indicate that this staged filling strategy increases available test time by roughly 20 % relative to single-stage filling of tailored driver gas mixtures, while simultaneously reducing the helium required per shock by up to 85 %. This filling scheme involves firstly mixing amore » tailored helium–nitrogen mixture in the driver section as in conventional driver filling and, secondly, backfilling a low-speed-of-sound gas such as nitrogen or carbon dioxide from a port close to the end cap of the driver section. Using this staged driver gas filling, in addition to the other techniques listed above, post-reflected shock test times of up to 0.102 s (102 ms) at 524 K and 1.6 atm have been obtained. Spectroscopically based temperature measurements in non-reactive mixtures have confirmed that temperature and pressure conditions remain constant throughout the length of these long test duration trials. Finally, these strategies have been used to measure low-temperature n-heptane ignition delay times.« less

High-Pressure Design of Advanced BN-Based Materials.

PubMed

Kurakevych, Oleksandr O; Solozhenko, Vladimir L

2016-10-20

The aim of the present review is to highlight the state of the art in high-pressure design of new advanced materials based on boron nitride. Recent experimental achievements on the governing phase transformation, nanostructuring and chemical synthesis in the systems containing boron nitride at high pressures and high temperatures are presented. All these developments allowed discovering new materials, e.g., ultrahard nanocrystalline cubic boron nitride (nano-cBN) with hardness comparable to diamond, and superhard boron subnitride B 13 N₂. Thermodynamic and kinetic aspects of high-pressure synthesis are described based on the data obtained by in situ and ex situ methods. Mechanical and thermal properties (hardness, thermoelastic equations of state, etc.) are discussed. New synthetic perspectives, combining both soft chemistry and extreme pressure-temperature conditions are considered.

Rapid Ovary Mass-Isolation (ROMi) to Obtain Large Quantities of Drosophila Egg Chambers for Fluorescent In Situ Hybridization.

PubMed

Jambor, Helena; Mejstrik, Pavel; Tomancak, Pavel

2016-01-01

Isolation of large quantities of tissue from organisms is essential for many techniques such as genome-wide screens and biochemistry. However, obtaining large quantities of tissues or cells is often the rate-limiting step when working in vivo. Here, we present a rapid method that allows the isolation of intact, single egg chambers at various developmental stages from ovaries of adult female Drosophila flies. The isolated egg chambers are amenable for a variety of procedures such as fluorescent in situ hybridization, RNA isolation, extract preparation, or immunostaining. Isolation of egg chambers from adult flies can be completed in 5 min and results, depending on the input amount of flies, in several milliliters of material. The isolated egg chambers are then further processed depending on the exact requirements of the subsequent application. We describe high-throughput in situ hybridization in 96-well plates as example application for the mass-isolated egg chambers.

Combined Theoretical and in Situ Scattering Strategies for Optimized Discovery and Recovery of High-Pressure Phases: A Case Study of the GaN–Nb 2O 5 System

DOE PAGES

Woerner, William R.; Qian, Guang-Rui; Oganov, Artem R.; ...

2016-03-22

The application of pressure in solid-state synthesis provides a route for the creation of new and exciting materials. However, the onerous nature of high-pressure techniques limits their utility in materials discovery. The systematic search for novel oxynitrides—semiconductors for photocatalytic overall water splitting—is a representative case where quench high-pressure synthesis is useful and necessary in order to obtain target compounds. In this paper, we utilize state of the art crystal structure prediction theory (USPEX) and in situ synchrotron-based X-ray scattering to speed up the discovery and optimization of novel compounds using high-pressure synthesis. Using this approach, two novel oxynitride phases weremore » discovered in the GaN–Nb 2O 5 system. The (Nb 2O 5) 0.84:(NbO 2) 0.32:(GaN) 0.82 rutile structured phase was formed at 1 GPa and 900°C and gradually transformed to a α-PbO 2-related structure above 2.8 GPa and 1000°C. The low-pressure rutile type phase was found to have a direct optical band gap of 0.84 eV and an indirect gap of 0.51 eV.« less

Combined Theoretical and in Situ Scattering Strategies for Optimized Discovery and Recovery of High-Pressure Phases: A Case Study of the GaN–Nb 2 O 5 System

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

Woerner, William R.; Qian, Guang-Rui; Oganov, Artem R.

2016-04-04

The application of pressure in solid-state synthesis provides a route for the creation of new and exciting materials. However, the onerous nature of high-pressure techniques limits their utility in materials discovery. The systematic search for novel oxynitrides—semiconductors for photocatalytic overall water splitting—is a representative case where quench high-pressure synthesis is useful and necessary in order to obtain target compounds. We utilize state of the art crystal structure prediction theory (USPEX) and in situ synchrotron-based X-ray scattering to speed up the discovery and optimization of novel compounds using high-pressure synthesis. Using this approach, two novel oxynitride phases were discovered in themore » GaN–Nb2O5 system. The (Nb2O5)0.84:(NbO2)0.32:(GaN)0.82 rutile structured phase was formed at 1 GPa and 900 °C and gradually transformed to a α-PbO2-related structure above 2.8 GPa and 1000 °C. The low-pressure rutile type phase was found to have a direct optical band gap of 0.84 eV and an indirect gap of 0.51 eV.« less

Bridging the pressure gap: In situ atomic-level investigations of model platinum catalyst surfaces under reaction conditions by scanning tunneling microscopy

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

McIntyre, Brian James

1994-05-01

Results of this thesis show that STM measurements can provide information about the surfaces and their adsorbates. Stability of Pt(110) under high pressures of H 2, O 2, and CO was studied (Chap. 4). In situ UHV and high vacuum experiments were carried out for sulfur on Pt(111) (Chap.5). STM studies of CO/S/Pt(111) in high CO pressures showed that the Pt substrate undergoes a stacking-fault-domain reconstruction involving periodic transitions from fcc to hcp stacking of top-layer atoms (Chap.6). In Chap.7, the stability of propylene on Pt(111) and the decomposition products were studied in situ with the HPSTM. Finally, in Chap.8,more » results are presented which show how the Pt tip of the HPSTM was used to locally rehydrogenate and oxidize carbonaceous clusters deposited on the Pt(111) surface; the Pt tip acted as a catalyst after activation by short voltage pulses.« less

In-situ neutron imaging of hydrogenous fuels in combustion generated porous carbons under dynamic and steady state pressure conditions

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

Ossler, Frederik; Santodonato, Louis J.; Bilheux, Hassina Z.

Here, we report results from experiments where we characterize the surface properties of soot particles interacting with high-pressure methane. We also found considerable differences in behavior of the soot material between static and dynamic pressure conditions that can be explained by multiscale correlations in the dynamics, from the micro to macro of the porous fractal-like carbon matrix. The measurements were possible utilizing cold neutron imaging of methane mixed with combustion generated carbon (soot) inside steel cells. The studies were performed under static and dynamic pressure conditions in the range 10-90 bar, and are of interest for applications of energy storagemore » of hydrogenous fuels. The very high cross sections for neutrons compared to hard X-ray photons, enabled us to find considerable amounts of native hydrogen in the soot and to see and quantify the presence of hydrogen atoms in the carbon soot matrix under different pressure conditions. Our work lays the base for more detailed in-situ investigations on the interaction of porous carbon materials with hydrogen in practical environments for hydrogen and methane storage.« less

In-situ neutron imaging of hydrogenous fuels in combustion generated porous carbons under dynamic and steady state pressure conditions

DOE PAGES

Ossler, Frederik; Santodonato, Louis J.; Bilheux, Hassina Z.

2017-02-12

Here, we report results from experiments where we characterize the surface properties of soot particles interacting with high-pressure methane. We also found considerable differences in behavior of the soot material between static and dynamic pressure conditions that can be explained by multiscale correlations in the dynamics, from the micro to macro of the porous fractal-like carbon matrix. The measurements were possible utilizing cold neutron imaging of methane mixed with combustion generated carbon (soot) inside steel cells. The studies were performed under static and dynamic pressure conditions in the range 10-90 bar, and are of interest for applications of energy storagemore » of hydrogenous fuels. The very high cross sections for neutrons compared to hard X-ray photons, enabled us to find considerable amounts of native hydrogen in the soot and to see and quantify the presence of hydrogen atoms in the carbon soot matrix under different pressure conditions. Our work lays the base for more detailed in-situ investigations on the interaction of porous carbon materials with hydrogen in practical environments for hydrogen and methane storage.« less

Micro X-ray CT imaging of pore-scale changes in unconsolidated sediment under confining pressure

NASA Astrophysics Data System (ADS)

Schindler, M.; Prasad, M.

2017-12-01

Micro X-ray computed tomography was used to image confining-pressure induced changes in a dry, unconsolidated quartz sand pack while simultaneously recording ultrasonic P-wave velocities. The experiments were performed under in-situ pressure of up to 4000 psi. The majority of digital rock physics studies rely on micro CT images obtained under ambient pressure and temperature conditions although effective rock properties strongly depend on in situ conditions. Goal of this work is to be able to obtain micro CT images of rock samples while pore and confining pressure is applied. Simultaneously we recorded ultrasonic P-wave velocities. The combination of imaging and velocity measurements provides insight in pore-scale changes in the rock and their influence on elastic properties. We visually observed a reduction in porosity by more than a third of the initial value as well as extensive grain damage, changes in pore and grain size distribution and an increase in contact number and contact radius with increasing confining pressure. An increase in measured ultrasonic P-wave velocities with increasing pressure was observed. We used porosity, contact number and contact radius obtained from micro CT images to model P-wave velocity with the contact-radius model by Bachrach et al. (1998). Our observations showed that the frame of unconsolidated sediments is significantly altered starting at pressures of only 1000 psi. This finding indicates that common assumptions in rock physics models (the solid frame remains unchanged) are violated for unconsolidated sediments. The effects on the solid frame should be taken into account when modeling the pressure dependence of elastic rock properties.

A Novel Telometric Metric for In-Situ Measurement of Intrauterine Pressure (IUP) in Pregnant and Parturient Rats

NASA Technical Reports Server (NTRS)

Baer, Lisa A.; LaFramboise, M. N.; Hills, E. M.; Daly, M. E.; Mills, N. A.; Wade, C. E.; Ronca, A. E.; Dalton, Bonnie (Technical Monitor)

2001-01-01

During labor and birth, considerable forces exerted on fetuses help instigate certain adaptive postpartum responses (viz., breathing and suckling). To make precise, reliable measures of the forces experienced by rat fetuses during parturition, we developed a novel method for measuring intrauterine pressure (IUP) in late pregnant rats. A small (1.25 x 4cm) telemetric blood pressure sensor is fitted within a fluid-filled balloon, similar in size to a full term rat fetus. The balloon is surgically implanted in the uterus on Gestational Day 19 of the rats' 22-day pregnancy. During birth, dams are able to deliver their pups and the balloon. IUP arsenals are recorded during labor (G22 or 23) and birth. Data derived from a group of implanted rats indicated that pressures on the balloon increased across the period of birth, reaching 18 mmHg during labor, 25 mmHg during pup births and 39 mmHg just prior to delivery of the balloon. These data are within the range reported for conventional IUP measurement techniques. Dams are simultaneously videotaped, enabling us to analyze behavioral expressions of labor contractions and to integrate in-situ and behavioral findings.

Comparison and verification of two models which predict minimum principal in situ stress from triaxial data

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

Harikrishnan, R.; Hareland, G.; Warpinski, N.R.

This paper evaluates the correlation between values of minimum principal in situ stress derived from two different models which use data obtained from triaxial core tests and coefficient for earth at rest correlations. Both models use triaxial laboratory tests with different confining pressures. The first method uses a vcrified fit to the Mohr failure envelope as a function of average rock grain size, which was obtained from detailed microscopic analyses. The second method uses the Mohr-Coulomb failure criterion. Both approaches give an angle in internal friction which is used to calculate the coefficient for earth at rest which gives themore » minimum principal in situ stress. The minimum principal in situ stress is then compared to actual field mini-frac test data which accurately determine the minimum principal in situ stress and are used to verify the accuracy of the correlations. The cores and the mini-frac stress test were obtained from two wells, the Gas Research Institute`s (GRIs) Staged Field Experiment (SFE) no. 1 well through the Travis Peak Formation in the East Texas Basin, and the Department of Energy`s (DOE`s) Multiwell Experiment (MWX) wells located west-southwest of the town of Rifle, Colorado, near the Rulison gas field. Results from this study indicates that the calculated minimum principal in situ stress values obtained by utilizing the rock failure envelope as a function of average rock grain size correlation are in better agreement with the measured stress values (from mini-frac tests) than those obtained utilizing Mohr-Coulomb failure criterion.« less

The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600.

PubMed

Burke, M G; Bertali, G; Prestat, E; Scenini, F; Haigh, S J

2017-05-01

In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. Copyright © 2016 Elsevier B.V. All rights reserved.

A method for measuring the local gas pressure within a gas-flow stage in situ in the transmission electron microscope

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

Colby, Robert J.; Alsem, Daan H.; Liyu, Andrey V.

2015-06-01

The development of environmental transmission electron microscopy (TEM) has enabled in situ experiments in a gaseous environment with high resolution imaging and spectroscopy. Addressing scientific challenges in areas such as catalysis, corrosion, and geochemistry can require pressures much higher than the ~20 mbar achievable with a differentially pumped, dedicated environmental TEM. Gas flow stages, in which the environment is contained between two semi-transparent thin membrane windows, have been demonstrated at pressures of several atmospheres. While this constitutes significant progress towards operando measurements, the design of many current gas flow stages is such that the pressure at the sample cannot necessarilymore » be directly inferred from the pressure differential across the system. Small differences in the setup and design of the gas flow stage can lead to very different sample pressures. We demonstrate a method for measuring the gas pressure directly, using a combination of electron energy loss spectroscopy and TEM imaging. This method requires only two energy filtered TEM images, limiting the measurement time to a few seconds and can be performed during an ongoing experiment at the region of interest. This approach provides a means to ensure reproducibility between different experiments, and even between very differently designed gas flow stages.« less

Field Aligned Currents Derived from Pressure Profiles Obtained from TWINS ENA Images

NASA Astrophysics Data System (ADS)

Wood, K.; Perez, J. D.; McComas, D. J.; Goldstein, J.; Valek, P. W.

2015-12-01

Field aligned currents (FACs) that flow from the Earth's magnetosphere into the ionosphere are an important coupling mechanism in the interaction of the solar wind with the Earth's magnetosphere. Assuming pressure balance along with charge conservation yields an expression for the FACs in terms of plasma pressure gradients and pressure anisotropy. The Two Wide-Angle Imaging Neutral Atom Spectrometers (TWINS) mission, the first stereoscopic ENA magnetospheric imager, provides global images of the inner magnetosphere from which ion pressure distributions and pressure anisotropies can be obtained. Following the formulations in Heineman [1990] and using results from TWINS observations, we calculate the distribution of field aligned currents for the 17-18 March 2015 geomagnetic storm in which extended ionospheric precipitation was observed. Initial results for the field aligned currents will be generated assuming an isotropic pitch angle distribution. Global maps of field aligned currents during the main and recovery phase of the storm will be presented. Heinemann, H. (1990), Representations of Currents and Magnetic Fields in Anisotropic Magnetohydrostatic Plasma, J. Geophys. Res., 95, 7789.

In-situ Diffraction Study of Magnetite at Simultaneous High Pressure and High Temperature Using Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Wang, L.; Zhang, J.; Wang, S.; Chen, H.; Zhao, Y.

2014-12-01

Magnetite intertwined with the evolution of human civilizations, and remains so today. It is technologically and scientifically important by virtue of its unique magnetic and electrical properties. Magnetite is a common mineral found in a variety of geologic environments, and plays an important role in deciphering the oxygen evolution in the Earth's atmosphere and its deep interiors. The latter application asks for the knowledge of the thermal and elastic properties of magnetite at high pressures and temperatures, which is currently not available in literature. We have carried out a few in-situ diffraction experiments on magnetite using white synchrotron radiation at beamline X17B2 of National Synchrotron Light Source (NSLS). A DIA module in an 1100-ton press and WC anvils were employed for compression, and diffraction spectra were collected at simultaneous high pressures (P) and temperatures (T) (up to 9 GPa and 900 oC). Mixture of amorphous boron and epoxy resin was used as pressure medium, and NaCl as pressure marker. Temperature was recorded by W-Re thermocouples. Commercially purchased magnetite powder and a mixture of the said powder and NaCl (1:1) were used as starting material in separate experiments. Preliminary data analyses have yielded following observations: (1) Charge disordering seen at ambient pressure remains active in current experiments, especially at lower pressures (< 6 GPa); (2) Though at each condition potentially complicated by charge disordering process, isothermal compression curves remains simple and reproducible; (3) During cooling, the reversibility and degree of cation disordering depend on the starting material and/or experimental P-T path; and (4) cation disordering notably reduces the apparent bulk moduli of magnetite.

Thermodynamic Pressure/Temperature Transducer Health Check

NASA Technical Reports Server (NTRS)

Immer, Christopher D. (Inventor); Eckhoff, Anthony (Inventor); Medelius, Pedro J. (Inventor); Deyoe, Richard T. (Inventor); Starr, Stanley O. (Inventor)

2004-01-01

A device and procedure for checking the health of a pressure transducer in situ is provided. The procedure includes measuring a fixed change in pressure above ambient pressure and a fixed change in pressure below ambient pressure. This is done by first sealing an enclosed volume around the transducer with a valve. A piston inside the sealed volume is increasing the pressure. A fixed pressure below ambient pressure is obtained by opening the valve, driving the piston The output of the pressure transducer is recorded for both the overpressuring and the underpressuring. By comparing this data with data taken during a preoperative calibration, the health of the transducer is determined from the linearity, the hysteresis, and the repeatability of its output. The further addition of a thermometer allows constant offset error in the transducer output to be determined.

Variability of in situ sediment strength and pore pressure behavior of tidal estuary surface sediments

NASA Astrophysics Data System (ADS)

Lucking, Greg; Stark, Nina; Lippmann, Thomas; Smyth, Stephen

2017-10-01

Tidal estuaries feature spatially and temporally varying sediment dynamics and characteristics. Particularly, the variability of geotechnical sediment parameters is still poorly understood, limiting the prediction of long-term sediment stability and dynamics. This paper presents results from an in situ investigation of surficial sediments (≤50 cm) in a tidal estuary in New Hampshire (USA), using a portable free fall penetrometer. The aim is to investigate variations in sediment strength and pore pressure behavior with regard to sediment type and seabed morphology. The study also provides a detailed analysis of high velocity impact pore pressure data to derive information about sediment type and permeability. The penetrometer was deployed 227 times, and the findings are correlated to 78 sediment samples. Differences in sediment strength and type were found when transitioning from tidal flats to the deeper channels. Finer-grained sediments located predominantly on the tidal flats appeared well consolidated with noticeable and spatially consistent sediment strength (reflected in an estimate of quasi-static bearing capacity qsbcmax 10 kPa). Sediments with higher sand content (>75%) showed more variations in strength relating to differences in gradation, and likely represent loose and poorly consolidated sands (qsbcmax 10-55 kPa). The rate at which the recorded excess pore pressures approached equilibrium after penetration was classified and related to sediment type. The data indicate that the development of excess pore pressures upon impact and during penetration may provide additional insight into the nature and layering of bed material, such as identifying a desiccated or over-consolidated dilative surficial layer. In summary, with varying sediment grain size distributions, bulk densities and morphology, sediment strength and pore pressure behavior can vary significantly within a tidal estuary.

Pollutant emissions from and within a model gas turbine combustor at elevated pressures and temperatures

NASA Technical Reports Server (NTRS)

Drennan, S. A.; Peterson, C. O.; Khatib, F. M.; Sowa, W. A.; Samuelsen, G. S.

1993-01-01

Conventional and advanced gas turbine engines are coming under increased scrutiny regarding pollutant emissions. This, in turn, has created a need to obtain in-situ experimental data at practical conditions, as well as exhaust data, and to obtain the data in combustors that reflect modern designs. The in-situ data are needed to (1) assess the effects of design modifications on pollutant formation, and (2) develop a detailed data base on combustor performance for the development and verification of computer modeling. This paper reports on a novel high pressure, high temperature facility designed to acquire such data under controlled conditions and with access (optical and extractive) for in-situ measurements. To evaluate the utility of the facility, a model gas turbine combustor was selected which features practical hardware design, two rows of jets (primary and dilution) with four jets in each row, and advanced wall cooling techniques with laser drilled effusive holes. The dome is equipped with a flat-vaned swirler with vane angles of 60 degrees. Data are obtained at combustor pressures ranging from 2 to 10 atmospheres of pressure, levels of air preheat to 427 C, combustor reference velocities from 10.0 to 20.0 m/s, and an overall equivalence ratio of 0.3. Exit plane and in-situ measurements are presented for HC, O2, CO2, CO, and NO(x). The exit plane emissions of NO(x) correspond to levels reported from practical combustors and the in-situ data demonstrate the utility and potential for detailed flow field measurements.

Improved Correction of Atmospheric Pressure Data Obtained by Smartphones through Machine Learning

PubMed Central

Kim, Yong-Hyuk; Ha, Ji-Hun; Kim, Na-Young; Im, Hyo-Hyuc; Sim, Sangjin; Choi, Reno K. Y.

2016-01-01

A correction method using machine learning aims to improve the conventional linear regression (LR) based method for correction of atmospheric pressure data obtained by smartphones. The method proposed in this study conducts clustering and regression analysis with time domain classification. Data obtained in Gyeonggi-do, one of the most populous provinces in South Korea surrounding Seoul with the size of 10,000 km2, from July 2014 through December 2014, using smartphones were classified with respect to time of day (daytime or nighttime) as well as day of the week (weekday or weekend) and the user's mobility, prior to the expectation-maximization (EM) clustering. Subsequently, the results were analyzed for comparison by applying machine learning methods such as multilayer perceptron (MLP) and support vector regression (SVR). The results showed a mean absolute error (MAE) 26% lower on average when regression analysis was performed through EM clustering compared to that obtained without EM clustering. For machine learning methods, the MAE for SVR was around 31% lower for LR and about 19% lower for MLP. It is concluded that pressure data from smartphones are as good as the ones from national automatic weather station (AWS) network. PMID:27524999

A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems

PubMed Central

Meyer, David; Prien, Ralf D.; Dellwig, Olaf; Waniek, Joanna J.; Schuffenhauer, Ingo; Donath, Jan; Krüger, Siegfried; Pallentin, Malte; Schulz-Bull, Detlef E.

2016-01-01

A METals In Situ analyzer (METIS) has been used to determine dissolved manganese (II) concentrations in the subhalocline waters of the Gotland Deep (central Baltic Sea). High-resolution in situ measurements of total dissolved Mn were obtained in near real-time by spectrophotometry using 1-(2-pyridylazo)-2-naphthol (PAN). PAN is a complexing agent of dissolved Mn and forms a wine-red complex with a maximum absorbance at a wavelength of 562 nm. Results are presented together with ancillary temperature, salinity, and dissolved O2 data. Lab calibration of the analyzer was performed in a pressure testing tank. A detection limit of 77 nM was obtained. For validation purposes, discrete water samples were taken by using a pump-CTD system. Dissolved Mn in these samples was determined by an independent laboratory based method (inductively coupled plasma–optical emission spectrometry, ICP-OES). Mn measurements from both METIS and ICP-OES analysis were in good agreement. The results showed that the in situ analysis of dissolved Mn is a powerful technique reducing dependencies on heavy and expensive equipment (pump-CTD system, ICP-OES) and is also cost and time effective. PMID:27916898

Feasibility of in situ, high-resolution correlation of tracer uptake with histopathology by quantitative autoradiography of biopsy specimens obtained under 18F-FDG PET/CT guidance.

PubMed

Fanchon, Louise M; Dogan, Snjezana; Moreira, Andre L; Carlin, Sean A; Schmidtlein, C Ross; Yorke, Ellen; Apte, Aditya P; Burger, Irene A; Durack, Jeremy C; Erinjeri, Joseph P; Maybody, Majid; Schöder, Heiko; Siegelbaum, Robert H; Sofocleous, Constantinos T; Deasy, Joseph O; Solomon, Stephen B; Humm, John L; Kirov, Assen S

2015-04-01

Core biopsies obtained using PET/CT guidance contain bound radiotracer and therefore provide information about tracer uptake in situ. Our goal was to develop a method for quantitative autoradiography of biopsy specimens (QABS), to use this method to correlate (18)F-FDG tracer uptake in situ with histopathology findings, and to briefly discuss its potential application. Twenty-seven patients referred for a PET/CT-guided biopsy of (18)F-FDG-avid primary or metastatic lesions in different locations consented to participate in this institutional review board-approved study, which complied with the Health Insurance Portability and Accountability Act. Autoradiography of biopsy specimens obtained using 5 types of needles was performed immediately after extraction. The response of autoradiography imaging plates was calibrated using dummy specimens with known activity obtained using 2 core-biopsy needle sizes. The calibration curves were used to quantify the activity along biopsy specimens obtained with these 2 needles and to calculate the standardized uptake value, SUVARG. Autoradiography images were correlated with histopathologic findings and fused with PET/CT images demonstrating the position of the biopsy needle within the lesion. Logistic regression analysis was performed to search for an SUVARG threshold distinguishing benign from malignant tissue in liver biopsy specimens. Pearson correlation between SUVARG of the whole biopsy specimen and average SUVPET over the voxels intersected by the needle in the fused PET/CT image was calculated. Activity concentrations were obtained using autoradiography for 20 specimens extracted with 18- and 20-gauge needles. The probability of finding malignancy in a specimen is greater than 50% (95% confidence) if SUVARG is greater than 7.3. For core specimens with preserved shape and orientation and in the absence of motion, one can achieve autoradiography, CT, and PET image registration with spatial accuracy better than 2 mm. The

High pressure in situ x-ray absorption spectroscopy cell for studying simultaneously the liquid phase and the solid-liquid interface

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

Grunwaldt, Jan-Dierk; Ramin, Michael; Rohr, Markus

2005-05-15

A high pressure in situ x-ray absorption spectroscopy cell with two different path lengths and path positions is presented for studying element-specifically both the liquid phase and the solid-liquid interface at pressures up to 250 bar and temperatures up to 220 deg. C. For this purpose, one x-ray path probes the bottom, while the other x-ray path penetrates through the middle of the in situ cell. The basic design of the cell resembles a 10 ml volume batch reactor, which is equipped with in- and outlet lines to dose compressed gases and liquids as well as a stirrer for goodmore » mixing. Due to the use of a polyetheretherketone inset it is also suitable for measurements under corrosive conditions. The characteristic features of the cell are illustrated using case studies from catalysis and solid state chemistry: (a) the ruthenium-catalyzed formylation of an amine in 'supercritical' carbon dioxide in the presence of hydrogen; (b) the cycloaddition of carbon dioxide to propylene oxide in the presence of a solid Zn-based catalyst, and (c) the solvothermal synthesis of MoO{sub 3} nanorods from MoO{sub 3}-2H{sub 2}O.« less

Compressibility and expansivity of anglesite (PbSO4) using in situ synchrotron X-ray diffraction at high-pressure and high-temperature conditions

NASA Astrophysics Data System (ADS)

Li, Bo; Xu, Jingui; Chen, Wei; Ye, Zhilin; Huang, Shijie; Fan, Dawei; Zhou, Wenge; Xie, Hongsen

2018-04-01

The compressibility and expansivity of anglesite (PbSO4) have been measured at high pressure up to 21.6 GPa and high temperature up to 700 K using in situ angle-dispersive X-ray diffraction and diamond anvil cell. The third-order Birch-Murnaghan equation of state (III-BM-EoS) was used to analyze the pressure-volume (P-V) data of PbSO4. We obtained the bulk modulus K 0 = 59(1) GPa, and its pressure derivative K0' = 5.3(4), respectively. Using Holland-Powell thermal EoS to fit the temperature-volume (T-V) data, the thermal expansion coefficient α 0 = 4.59(2) × 10- 5 K- 1 for PbSO4 was also derived. Simultaneously, the ambient-pressure axial compressibilities (β a0 = 1.79(4) × 10- 3 GPa- 1, β b0 = 1.75(5) × 10- 3 GPa- 1, β c0 = 2.12(4) × 10- 3 GPa- 1) and axial thermal expansivities (α a0 = 1.23(4) × 10- 5 K- 1, α b0 = 1.93(2) × 10- 5 K- 1, and α c0 = 1.43(1) × 10- 5 K- 1) along a-axis, b-axis and c-axis were derived at 300 K, respectively. Furthermore, the potential influencing factors (e.g., the effective size of M2+ cation, polarizability and electronegativity) on the bulk moduli of barite-type (belonging to Pbnm space group) sulfates (anglesite, barite, and celestine) were discussed. We found that the polarizability might be the most important factor. Finally, the anisotropic linear compressibility and thermal expansivity in barite-type sulfates were also discussed, respectively.

Effect of confining pressure on diffusion coefficients in clay-rich, low-permeability sedimentary rocks.

PubMed

Xiang, Y; Al, T; Mazurek, M

2016-12-01

The effect of confining pressure (CP) on the diffusion of tritiated-water (HTO) and iodide (I - ) tracers through Ordovician rocks from the Michigan Basin, southwestern Ontario, Canada, and Opalinus Clay from Schlattingen, Switzerland was investigated in laboratory experiments. Four samples representing different formations and lithologies in the Michigan Basin were studied: Queenston Formation shale, Georgian Bay Formation shale, Cobourg Formation limestone and Cobourg Formation argillaceous limestone. Estimated in situ vertical stresses at the depths from which the samples were retrieved range from 12.0 to 17.4MPa (Michigan Basin) and from 21 to 23MPa (Opalinus Clay). Effective diffusion coefficients (D e ) were determined in through-diffusion experiments. With HTO tracer, applying CP resulted in decreases in D e of 12.5% for the Queenston Formation shale (CP max =12MPa), 30% for the Georgian Bay Formation shale (15MPa), 34% for the Cobourg Formation limestone (17.4MPa), 31% for the Cobourg Formation argillaceous limestone (17.4MPa) and 43-46% for the Opalinus Clay (15MPa). Decreases in D e were larger for the I - tracer: 13.8% for the Queenston shale, 42% for the Georgian Bay shale, 50% for the Cobourg Formation limestone, 55% for the Cobourg Formation argillaceous limestone and 63-68% for the Opalinus Clay. The tracer-specific nature of the response is attributed to an increasing influence of anion exclusion as the pore size decreases at higher CP. Results from the shales (including Opalinus Clay) indicate that the pressure effect on D e can be represented by a linear relationship between D e and ln(CP), which provides valuable predictive capability. The nonlinearity results in a relatively small change in D e at high CP, suggesting that it is not necessary to apply the exact in situ pressure conditions in order to obtain a good estimate of the in situ diffusion coefficient. Most importantly, the CP effect on shale is reversible (±12%) suggesting that, for

Silicate Carbonation in Supercritical CO2 Containing Dissolved H2O: An in situ High Pressure X-Ray Diffraction Study

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

Schaef, Herbert T.; Miller, Quin RS; Thompson, Christopher J.

2013-06-30

Technological advances have been significant in recent years for managing environmentally harmful emissions (mostly CO2) resulting from combustion of fossil fuels. Deep underground geologic formations are emerging as reasonable options for long term storage of CO2 but mechanisms controlling rock and mineral stability in contact with injected supercritical fluids containing water are relatively unknown. In this paper, we discuss mineral transformation reactions occurring between supercritical CO2 containing water and the silicate minerals forsterite (Mg2SiO4), wollastonite (CaSiO3), and enstatite (MgSiO3). This study utilizes newly developed in situ high pressure x-ray diffraction (HXRD) and in situ infra red (IR) to examine mineralmore » transformation reactions. Forsterite and enstatite were selected as they are important minerals present in igneous and mafic rocks and have been the subject of a large number of aqueous dissolution studies that can be compared with non-aqueous fluid tests in this study. Wollastonite, classified as a pyroxenoid (similar to a pyroxene), was chosen as a suitably fast reacting proxy for examining silicate carbonation processes associated with a wet scCO2 fluid as related to geologic carbon sequestration. The experiments were conducted under modest pressures (90 to 160 bar), temperatures between 35° to 70° C, and varying concentrations of dissolved water. Under these conditions scCO2 contains up to 3,500 ppm dissolved water.« less

Characterization of cavity flow fields using pressure data obtained in the Langley 0.3-Meter Transonic Cryogenic Tunnel

NASA Technical Reports Server (NTRS)

Tracy, M. B.; Plentovich, E. B.

1993-01-01

Static and fluctuating pressure distributions were obtained along the floor of a rectangular-box cavity in an experiment performed in the LaRC 0.3-Meter Transonic Cryogenic Tunnel. The cavity studied was 11.25 in. long and 2.50 in. wide with a variable height to obtain length-to-height ratios of 4.4, 6.7, 12.67, and 20.0. The data presented herein were obtained for yaw angles of 0 deg and 15 deg over a Mach number range from 0.2 to 0.9 at a Reynolds number of 30 x 10(exp 6) per ft with a boundary-layer thickness of approximately 0.5 in. The results indicated that open and transitional-open cavity flow supports tone generation at subsonic and transonic speeds at Mach numbers of 0.6 and above. Further, pressure fluctuations associated with acoustic tone generation can be sustained when static pressure distributions indicate that transitional-closed and closed flow fields exist in the cavity. Cavities that support tone generation at 0 deg yaw also supported tone generation at 15 deg yaw when the flow became transitional-closed. For the latter cases, a reduction in tone amplitude was observed. Both static and fluctuating pressure data must be considered when defining cavity flow fields, and the flow models need to be refined to accommodate steady and unsteady flows.

Melting diagrams of Fe-rich alloys determined from synchrotron in situ measurements in the 15-23 GPa pressure range

NASA Astrophysics Data System (ADS)

Andrault, D.; Bolfan-Casanova, N.; Ohtaka, O.; Fukui, H.; Arima, H.; Fialin, M.; Funakoshi, K.

2009-05-01

We report in situ observations of the melting behaviour of iron alloyed with 10-20 at.% C, O, S, or Si at pressures between 15 and 24 GPa, using X-ray diffraction in a multi-anvil press (SPring8). The degree of partial melting of the iron alloys has been quantified from analysis of the intensity of diffuse X-ray scattering of molten iron as a function for decreasing temperature with a 50° step. Coupled with microanalysis of recovered samples, the in situ observations bring direct constraints on shape and positions of liquidus and solidus curves in the melting diagrams. For the Fe-S system, our results are in good agreement with previous works. We observe that the eutectic temperature increases from 1023 K at 15 GPa to 1123 K at 20.6 GPa and that the eutectic composition decreases with increases pressure. Concerning the Fe-C system the eutectic temperature of 1460 K at 20.7 GPa falls slightly below a linear extrapolation of the previous work. In the case of the Fe-Ni-Si system and the Fe-O system, we find eutectic temperatures significantly lower than previously reported. For the two systems, both eutectic temperature and composition increase with increasing pressure in the 15-20 GPa range. Compare to previous work, we observe eutectic compositions (a) richer in light elements in the Fe-O system, with 9.0 and 10.5 wt% O at 16.5 and 20.5 GPa, respectively, and (b) poorer in the Fe-Ni-Si system with 11.5 wt% Si at 16.9 GPa. We confirm very high solubility of Si and C with solid iron, and report a Si partitioning coefficient of 1.3(2) at 16.9 GPa. The S and O solubility in solid iron appears very small. Therefore, both S and/or O could explain density jumps between liquid outer and solid inner parts of planetary cores, at least up to ˜25 GPa.

PETher - Physical Properties of Thermal Water under In-situ-Conditions

NASA Astrophysics Data System (ADS)

Herfurth, Sarah; Schröder, Elisabeth

2016-04-01

designed in-house to meet any geothermal reservoir conditions present in Germany. The obtained results will be compared with standard analytical methods as well as used to calibrate laboratory measurements that simulate the encountered in-situ conditions. A series of measurements will be performed to create a data base. In addition, these data can be used as reference data for developing and validating numerical models. In-situ measurements - in contrast to laboratory measurements - record the data online and instantaneously during normal operation of the plant and without changing the properties of the investigated fluid (pressure, temperature, etc.). Due to this, the uncertainties in the thermo-physical properties caused by degassing and precipitation are studiously avoided. As a result, the thermo-physical properties density, specific isobaric heat capacity, kinematic viscosity and thermal conductivity have been measured as functions of the geothermal water temperature, pressure and salinity at five sites, up to now. The measurements show that the thermo-physical properties correlate strongly with the salinity and therefore differ considerably from pure water values when a significant salt content is present.

In situ respiration measurements of megafauna in the Kermadec Trench

NASA Astrophysics Data System (ADS)

Nunnally, Clifton C.; Friedman, Jason R.; Drazen, Jeffrey C.

2016-12-01

The aim of this paper is to measure metabolic rates of megafauna living in depths greater than 6000 m. Echinoderms, actinarians and a polychaete were captured by remotely operated vehicle (ROV) and inserted into respiration chambers in situ at depths of 4049 m, 7140 m and 8074 m in the region of the Kermadec Trench SW Pacific Ocean. Hadal research has moved into a new frontier as technological improvements now allow for a meticulous investigation of trench ecology in depths greater than 6000 m. The development of an in situ respirometer for use in these studies was deployed in the Kermadec Trench to obtain the first ever rates of basal metabolic rates of hadal megafauna. Typical deep-sea experiments of individual animal physiology must deal with covarying factors of pressure, temperature, light and food supply in this study investigated the effects of pressure and increased food supply on overall animal metabolism. In the Kermadec Trench, holothurian respiration rates (n=4), 0.079±0.011 (mean±SE) μmol-O2 g-1 h-1, were higher than those captured at abyssal depths (n=2), 0.018±0.002 μmol-O2 g-1h-1, in the same region (p<0.001). When Q10 adjusted to a common temperature of 2.5 °C trench holothurian respiration rates ranged between 0.068 and 0.119 μmol-O2 g-1 h-1. Anemone respiration rates were remarkably similar between abyssal and hadal specimens, 0.110 and 0.111 μmol-O2 g-1 h-1, respectively. Our results on echinoderm respiration when corrected for temperature and mass fall below the slope regression when compared with other in situ measurements at shallower ocean depths.

An internally consistent pressure calibration of geobarometers applicable to the Earth’s upper mantle using in situ XRD

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

Beyer, Christopher; Rosenthal, Anja; Myhill, Robert

We have performed an experimental cross calibration of a suite of mineral equilibria within mantle rock bulk compositions that are commonly used in geobarometry to determine the equilibration depths of upper mantle assemblages. Multiple barometers were compared simultaneously in experimental runs, where the pressure was determined using in-situ measurements of the unit cell volumes of MgO, NaCl, Re and h-BN between 3.6 and 10.4 GPa, and 1250 and 1500 °C. The experiments were performed in a large volume press (LVPs) in combination with synchrotron X-ray diffraction. Noble metal capsules drilled with multiple sample chambers were loaded with a range ofmore » bulk compositions representative of peridotite, eclogite and pyroxenite lithologies. By this approach, we simultaneously calibrated the geobarometers applicable to different mantle lithologies under identical and well determined pressure and temperature conditions. We identified discrepancies between the calculated and experimental pressures for which we propose simple linear or constant correction factors to some of the previously published barometric equations. As a result, we establish internally-consistent cross-calibrations for a number of garnet-orthopyroxene, garnet-clinopyroxene, Ca-Tschermaks-in-clinopyroxene and majorite geobarometers.« less

Martian tidal pressure and wind fields obtained from the Mariner 9 infrared spectroscopy experiment

NASA Technical Reports Server (NTRS)

Pirraglia, J. A.; Conrath, B. J.

1973-01-01

Using temperature fields derived from the Mariner 9 infrared spectroscopy experiment, the Martian atmospheric tidal pressure and wind fields are calculated. Temperature as a function of local time, latitude, and atmospheric pressure level is obtained by secular and longitudinal averaging of the data. The resulting temperature field is approximated by a spherical harmonic expansion, retaining one symmetric and one asymmetric term for wavenumber zero and wavenumber one. Vertical averaging of the linearized momentum and continuity equations results in an inhomogeneous tidal equation for surface pressure fluctuations with the driving function related to the temperature field through the geopotential function and the hydrostatic equation. Solutions of the tidal equation show a diurnal fractional pressure amplitude approximately equal to one half of the vertically averaged diurnal fractional temperature amplitude.

Martian tidal pressure and wind fields obtained from the Mariner 9 infrared spectroscopy experiment

NASA Technical Reports Server (NTRS)

Pirraglia, J. A.; Conrath, B. J.

1974-01-01

Using temperature fields derived from the Mariner 9 infrared spectroscopy experiment, the Martian atmospheric tidal pressure and wind fields are calculated. Temperature as a function of local time, latitude, and atmospheric pressure level is obtained by secular and longitudinal averaging of the data. The resulting temperature field is approximated by a spherical harmonic expansion, retaining one symmetric and one asymmetric term each for wavenumber zero and wavenumber one. Vertical averaging of the linearized momentum and continuity equations results in an inhomogeneous tidal equation for surface pressure fluctuations with the driving function related to the temperature field through the geopotential function and the hydrostatic equation. Solutions of the tidal equation show a diurnal fractional pressure amplitude approximately equal to one-half the vertically averaged diurnal fractional temperature amplitude.

Trends in high pressure developments for new perspectives

NASA Astrophysics Data System (ADS)

Largeteau, Alain; Prakasam, Mythili

2018-06-01

Temperature and Pressure are two parameters in the universe, where pressure represents the largest scale in comparison to temperature. The design of high pressure equipment depends mainly on the media used which could be gas, liquid or solid and the objective could be synthesis of materials or in situ characterization. The development of new research fields requiring high pressure equipment which are currently in Bordeaux - France are based on the historical development of high pressure domain initiated by Professor Gerard DEMAZEAU and his team during the last half century, which is discussed here. The main concepts governing the effect of pressure on materials synthesis is by the combination of high pressure and high temperature which are described with apt examples. There is an upsurge in various technologies for strong development for the synthesis of materials to drive several possibilities, for example: to reach very high density to obtain optical ceramics (by conventional SPS), to diminish parameters (P, T, t) of synthesis (by HP-SPS), to sinter at low temperature thermal sensitive composition (by HyS), to consolidate porous materials (by FIP), to densify biocomposite with cold decontamination (by HHP) simultaneously, etc.

Development of in situ CO2 and pH sensor for AUVs and ROVs

NASA Astrophysics Data System (ADS)

Nakano, Yoshiyuki; Kimoto, Hideshi; Miwa, Tetsuya; Yoshida, Hiroshi

2013-04-01

Japan Agency for Marine-Earth Science and Technology (JAMSTEC) has been developing two-type autonomous underwater vehicles (AUVs): a cruising AUV and a working AUV, since October 2010. These vehicles will perform carbon dioxide (CO2) and pH observations to explore hydrothermal plume on seabed mineral resources and to monitor a leak of CO2 in carbon capture and storage (CCS) up to depth of 3,000 meters. We here have been developing the compact in situ CO2 and pH sensor (Hybrid CO2-pH sensor: HCS) for the AUVs to obtain vertical and horizontal distributions of CO2 and pH. The HCS consists of an aluminum pressure housing (diameter 84 mm, length 570 mm, weight 4 kg) and an acrylic silicon-oil filled, pressure-compensated vessel (diameter 90 mm, length 355 mm, weight 2 kg) containing valves and pump unit. The HCS is also useful for the observation by remotely operated vehicles (ROVs). The measured data were transmitted to the AUVs or ROVs by serial communications. We can monitor the data of in situ pCO2, pH and so on in real time on board. The measurement principle for the CO2 sensor is based on spectrophotometry. The pCO2 is calculated from the optical absorbance of the pH indicator solution equilibrated with CO2 in seawater through a gas permeable membrane. On the other hand, we adopt potentiometric analysis using original glass and reference electrodes as a pH sensor because of the most commonly used technique for sea water pH measurements and high-speed response (within 20 seconds). From simultaneously measured data of in situ pCO2 and pH, we can also calculate dissolved inorganic carbon (DIC) and total alkalinity (TA) as other carbonate species in the ocean. The resolutions of HCS are 1 μatm for pCO2 and 0.001 pH. In the laboratory experiment, the HCS obtained precisions within 3 μatm and within 0.01 pH, respectively. Our first in situ observational test of the HSC with cruising AUV was made in the coast of the Japan Sea last August. And also first in situ test

A Differential Pressure Instrument with Wireless Telemetry for In-Situ Measurement of Fluid Flow across Sediment-Water Boundaries

PubMed Central

Gardner, Alan T.; Karam, Hanan N.; Mulligan, Ann E.; Harvey, Charles F.; Hammar, Terence R.; Hemond, Harold F.

2009-01-01

An instrument has been built to carry out continuous in-situ measurement of small differences in water pressure, conductivity and temperature, in natural surface water and groundwater systems. A low-cost data telemetry system provides data on shore in real time if desired. The immediate purpose of measurements by this device is to continuously infer fluxes of water across the sediment-water interface in a complex estuarine system; however, direct application to assessment of sediment-water fluxes in rivers, lakes, and other systems is also possible. Key objectives of the design include both low cost, and accuracy of the order of ±0.5 mm H2O in measured head difference between the instrument's two pressure ports. These objectives have been met, although a revision to the design of one component was found to be necessary. Deployments of up to nine months, and wireless range in excess of 300 m have been demonstrated. PMID:22389608

Reproducibility and interoperator reliability of obtaining images and measurements of the cervix and uterus with brachytherapy treatment applicators in situ using transabdominal ultrasound.

PubMed

van Dyk, Sylvia; Garth, Margaret; Oates, Amanda; Kondalsamy-Chennakesavan, Srinivas; Schneider, Michal; Bernshaw, David; Narayan, Kailash

2016-01-01

To validate interoperator reliability of brachytherapy radiation therapists (RTs) in obtaining an ultrasound image and measuring the cervix and uterine dimensions using transabdominal ultrasound. Patients who underwent MRI with applicators in situ after the first insertion were included in the study. Imaging was performed by three RTs (RT1, RT2, and RT3) with varying degrees of ultrasound experience. All RTs were required to obtain a longitudinal planning image depicting the applicator in the uterine canal and measure the cervix and uterus. The MRI scan, taken 1 hour after the ultrasound, was used as the reference standard against which all measurements were compared. Measurements were analyzed with intraclass correlation coefficient and Bland-Altman plots. All RTs were able to obtain a suitable longitudinal image for each patient in the study. Mean differences (SD) between MRI and ultrasound measurements obtained by RTs ranged from 3.5 (3.6) to 4.4 (4.23) mm and 0 (3.0) to 0.9 (2.5) mm on the anterior and posterior surface of the cervix, respectively. Intraclass correlation coefficient for absolute agreement between MRI and RTs was >0.9 for all posterior measurement points in the cervix and ranged from 0.41 to 0.92 on the anterior surface. Measurements were not statistically different between RTs at any measurement point. RTs with variable training attained high levels of interoperator reliability when using transabdominal ultrasound to obtain images and measurements of the uterus and cervix with brachytherapy applicators in situ. Access to training and use of a well-defined protocol assist in achieving these high levels of reliability. Copyright © 2016 American Brachytherapy Society. Published by Elsevier Inc. All rights reserved.

Self-Calibrating Pressure Transducer

NASA Technical Reports Server (NTRS)

Lueck, Dale E. (Inventor)

2006-01-01

A self-calibrating pressure transducer is disclosed. The device uses an embedded zirconia membrane which pumps a determined quantity of oxygen into the device. The associated pressure can be determined, and thus, the transducer pressure readings can be calibrated. The zirconia membrane obtains oxygen .from the surrounding environment when possible. Otherwise, an oxygen reservoir or other source is utilized. In another embodiment, a reversible fuel cell assembly is used to pump oxygen and hydrogen into the system. Since a known amount of gas is pumped across the cell, the pressure produced can be determined, and thus, the device can be calibrated. An isolation valve system is used to allow the device to be calibrated in situ. Calibration is optionally automated so that calibration can be continuously monitored. The device is preferably a fully integrated MEMS device. Since the device can be calibrated without removing it from the process, reductions in costs and down time are realized.

Diagnostics of plasma-biological surface interactions in low pressure and atmospheric pressure plasmas

NASA Astrophysics Data System (ADS)

Ishikawa, Kenji; Hori, Masaru

2014-08-01

Mechanisms of plasma-surface interaction are required to understand in order to control the reactions precisely. Recent progress in atmospheric pressure plasma provides to apply as a tool of sterilization of contaminated foodstuffs. To use the plasma with safety and optimization, the real time in situ detection of free radicals - in particular dangling bonds by using the electron-spin-resonance (ESR) technique has been developed because the free radical plays important roles for dominantly biological reactions. First, the kinetic analysis of free radicals on biological specimens such as fungal spores of Penicillium digitatum interacted with atomic oxygen generated plasma electric discharge. We have obtained information that the in situ real time ESR signal from the spores was observed and assignable to semiquinone radical with a g-value of around 2.004 and a line width of approximately 5G. The decay of the signal was correlated with a link to the inactivation of the fungal spore. Second, we have studied to detect chemical modification of edible meat after the irradiation. Using matrix-assisted laser desorption/ionization time-of-flight mass spectroscopy (MALDI-TOF-MS) and ESR, signals give qualification results for chemical changes on edible liver meat. The in situ real-time measurements have proven to be a useful method to elucidate plasma-induced surface reactions on biological specimens.

Embedding Piezoresistive Pressure Sensors to Obtain Online Pressure Profiles Inside Fiber Composite Laminates

PubMed Central

Kahali Moghaddam, Maryam; Breede, Arne; Brauner, Christian; Lang, Walter

2015-01-01

The production of large and complex parts using fiber composite materials is costly due to the frequent formation of voids, porosity and waste products. By embedding different types of sensors and monitoring the process in real time, the amount of wastage can be significantly reduced. This work focuses on developing a knowledge-based method to improve and ensure complete impregnation of the fibers before initiation of the resin cure. Piezoresistive and capacitive pressure sensors were embedded in fiber composite laminates to measure the real-time the pressure values inside the laminate. A change of pressure indicates resin infusion. The sensors were placed in the laminate and the resin was infused by vacuum. The embedded piezoresistive pressure sensors were able to track the vacuum pressure in the fiber composite laminate setup, as well as the arrival of the resin at the sensor. The pressure increase due to closing the resin inlet was also measured. In contrast, the capacitive type of sensor was found to be inappropriate for measuring these quantities. The following study demonstrates real-time monitoring of pressure changes inside the fiber composite laminate, which validate the use of Darcy’s law in porous media to control the resin flow during infusion. PMID:25825973

Embedding piezoresistive pressure sensors to obtain online pressure profiles inside fiber composite laminates.

PubMed

Moghaddam, Maryam Kahali; Breede, Arne; Brauner, Christian; Lang, Walter

2015-03-27

The production of large and complex parts using fiber composite materials is costly due to the frequent formation of voids, porosity and waste products. By embedding different types of sensors and monitoring the process in real time, the amount of wastage can be significantly reduced. This work focuses on developing a knowledge-based method to improve and ensure complete impregnation of the fibers before initiation of the resin cure. Piezoresistive and capacitive pressure sensors were embedded in fiber composite laminates to measure the real-time the pressure values inside the laminate. A change of pressure indicates resin infusion. The sensors were placed in the laminate and the resin was infused by vacuum. The embedded piezoresistive pressure sensors were able to track the vacuum pressure in the fiber composite laminate setup, as well as the arrival of the resin at the sensor. The pressure increase due to closing the resin inlet was also measured. In contrast, the capacitive type of sensor was found to be inappropriate for measuring these quantities. The following study demonstrates real-time monitoring of pressure changes inside the fiber composite laminate, which validate the use of Darcy's law in porous media to control the resin flow during infusion.

Pressure-temperature gelatinization phase diagram of starch: An in situ Fourier transform infrared study.

PubMed

Rubens, P; Heremans, K

2000-12-01

The gelatinization of rice starch is reported as a function of temperature and pressure from the changes in the ir spectrum. The diagram that is observed is reminiscent of those obtained for the denaturation of proteins and the phase separation observed from the cloud point for several water soluble synthetic polymers. It is proposed that the reentrant shape of the diagram for starch is not only due to hydrogen bonding but also to the imperfect packing of amylose and amylopectin chains in the starch granule. The influence of pressure and temperature on thermodynamic parameters leading to this diagram is discussed. Copyright 2000 John Wiley & Sons, Inc.

Characterization of Gas-Hydrate Sediment: In Situ Evaluation of Hydrate Saturation in Pores of Pressured Sedimental Samples

NASA Astrophysics Data System (ADS)

Jin, Y.; Konno, Y.; Kida, M.; Nagao, J.

2014-12-01

Hydrate saturation of gas-hydrate bearing sediment is a key of gas production from natural gas-hydrate reservoir. Developable natural gas-hydrates by conventional gas/oil production apparatus almost exist in unconsolidated sedimental layer. Generally, hydrate saturations of sedimental samples are directly estimated by volume of gas generated from dissociation of gas hydrates in pore spaces, porosity data and volume of the sediments. Furthermore, hydrate saturation can be also assessed using velocity of P-wave through sedimental samples. Nevertheless, hydrate saturation would be changed by morphological variations (grain-coating, cementing and pore-filling model) of gas hydrates in pore spaces. Jin et al.[1,2] recently observed the O-H stretching bands of H2O molecules of methane hydrate in porous media using an attenuated total reflection IR (ATR-IR) spectra. They observed in situ hydrate formation/dissociation process in sandy samples (Tohoku Keisya number 8, grain size of ca. 110 μm). In this presentation, we present IR spectroscopy approach to in situ evaluation of hydrate saturation of pressured gas-hydrate sediments. This work was supported by funding from the Research Consortium for Methane Hydrate Resources in Japan (MH21 Research Consortium) planned by the Ministry of Economy, Trade and Industry (METI), Japan. [1] Jin, Y.; Konno, Y.; Nagao, J. Energy Fules, 2012, 26, 2242-2247. [2] Jin, Y.; Oyama, H.; Nagao, J. Jpn. J. Appl. Phys. 2009, 48, No. 108001.

Comparison of biodiesel production from sewage sludge obtained from the A²/O and MBR processes by in situ transesterification.

PubMed

Qi, Juanjuan; Zhu, Fenfen; Wei, Xiang; Zhao, Luyao; Xiong, Yiqun; Wu, Xuemin; Yan, Fawei

2016-03-01

The potential of two types of sludge obtained from the anaerobic-anoxic-oxic (A(2)/O) and membrane bioreactor (MBR) processes as lipid feedstock for biodiesel production via in situ transesterification was investigated. Experiments were conducted to determine the optimum conditions for biodiesel yield using three-factor and four-level orthogonal and single-factor tests. Several factors, namely, methanol-to-sludge mass ratio, acid concentration, and temperature, were examined. The optimum yield of biodiesel (16.6% with a fatty acid methyl ester purity of 96.7%) from A(2)/O sludge was obtained at a methanol-to-sludge mass ratio of 10:1, a temperature of 60°C, and a H2SO4 concentration of 5% (v/v). Meanwhile, the optimum yield of biodiesel (4.2% with a fatty acid methyl ester purity of 92.7%) from MBR sludge was obtained at a methanol-to-sludge mass ratio of 8:1, a temperature of 50°C, and a H2SO4 concentration of 5% (v/v). In this research, A(2)/O technology with a primary sedimentation tank is more favorable for obtaining energy from wastewater than MBR technology. Copyright © 2016 Elsevier Ltd. All rights reserved.

Cryogenic System for Neutron Scattering Experiments with In Situ Pressure Tuning Mechanism: Response of the Antiferromagnetism of URu2Si2 to Uniaxial Stress

NASA Astrophysics Data System (ADS)

Kawarazaki, Shuzo; Uwatoko, Yoshiya; Yokoyama, Makoto; Okita, Yuji; Tabata, Yoshikazu; Taniguchi, Toshifumi; Amitsuka, Hiroshi

2002-10-01

A handy insertable device to manipulate hydrostatic pressure or uniaxial stress on a sample in a cryostat for neutron scattering experiments is described. The pressure that is generated in a miniature hydraulic oil-cylinder on the top of the inserting stick is transmitted to the sample via a long piston-cylinder unit made of a thick stainless-steel tube and a fiber-reinforced plastics (FRP) rod. One can thus in situ tune the pressure or the stress on the sample without handling the pressure-cell at room temperature outside the cryostat. The device is designed to fit into the ILL-type Orange cryostat so that it can be used in many neutron scattering facilities. A newly designed uniaxial-stress cell and hydrostatic pressure cell to be used with this system are also described. The result of measurement of the hysteresis effect of uniaxial stress on the antiferromagnetism of URu2Si2 at 1.4 K is presented.

In situ measurement of tritium permeation through stainless steel

NASA Astrophysics Data System (ADS)

Luscher, Walter G.; Senor, David J.; Clayton, Kevin K.; Longhurst, Glen R.

2013-06-01

The TMIST-2 irradiation experiment was conducted in the Advanced Test Reactor at Idaho National Laboratory to evaluate tritium permeation through Type 316 stainless steel (316 SS). The interior of a 316 SS seamless tube specimen was exposed to a 4He carrier gas mixed with a specified quantity of tritium (T2) to yield partial pressures of 0.1, 5, and 50 Pa at 292 °C and 330 °C. In situ tritium permeation measurements were made by passing a He-Ne sweep gas over the outer surface of the specimen to carry the permeated tritium to a bubbler column for liquid scintillation counting. Results from in situ permeation measurements were compared with predictions based on an ex-reactor permeation correlation in the literature. In situ permeation data were also used to derive an in-reactor permeation correlation as a function of temperature and pressure over the ranges considered in this study. In addition, the triton recoil contribution to tritium permeation, which results from the transmutation of 3He to T, was also evaluated by introducing a 4He carrier gas mixed with 3He at a partial pressure of 1013 Pa at 330 °C. Less than 3% of the tritium resulting from 3He transmutation contributed to tritium permeation.

In situ CF3 Detection in Low Pressure Inductive Discharges by Fourier Transform Infrared Spectroscopy

NASA Technical Reports Server (NTRS)

Kim, J. S.; Cappelli, M. A.; Sharma, S. P.; Arnold, J. O. (Technical Monitor)

1998-01-01

The detection of CF(x) (x=1-3) radicals in low pressure discharges using source gases such as CF4 and CHF3 is of importance to the understanding of their chemical structure and relevance in plasma based etching processes. These radicals are known to contribute to the formation of fluorocarbon polymer films, which affect the selectivity and anisotropy of etching. In this study, we present preliminary results of the quantitative measurement of trifluoromethyl radicals, CF3, in low pressure discharges. The discharge studied here is an inductively (transformer) coupled plasma (ICP) source in the GEC reference cell, operating on pure CF4 at pressures ranging from 10 - 100 mTorr, This plasma source generates higher electron number densities at lower operating pressures than obtainable with the parallel-plate capacitively coupled version of the GEC reference cell. Also, this expanded operating regime is more relevant to new generations of industrial plasma reactors being used by the microelectronics industry. Fourier transform infrared (FTIR) spectroscopy is employed to observe the absorption band of CF3 radicals in the electronic ground state X2Al in the region of 1233-1270/cm. The spectrometer is equipped with a high sensitivity HgCdTe (MCT) detector and has a fixed resolution of 0.125/cm. The CF3 concentrations are measured for a range of operating pressures and discharge power levels.

Detailed pressure distribution measurements obtained on several configurations of an aspect-ratio-7 variable twist wing

NASA Technical Reports Server (NTRS)

Holbrook, G. T.; Dunham, D. M.

1985-01-01

Detailed pressure distribution measurements were made for 11 twist configurations of a unique, multisegmented wing model having an aspect ratio of 7 and a taper ratio of 1. These configurations encompassed span loads ranging from that of an untwisted wing to simple flapped wings both with and without upper-surface spoilers attached. For each of the wing twist configurations, electronic scanning pressure transducers were used to obtain 580 surface pressure measurements over the wing in about 0.1 sec. Integrated pressure distribution measurements compared favorably with force-balance measurements of lift on the model when the model centerbody lift was included. Complete plots and tabulations of the pressure distribution data for each wing twist configuration are provided.

Small-scale Pressure-balanced Structures Driven by Oblique Slow Mode Waves Measured in the Solar Wind

NASA Astrophysics Data System (ADS)

Yao, Shuo; He, J.-S.; Tu, C.-Y.; Wang, L.-H.; Marsch, E.

2013-09-01

Recently, small-scale pressure-balanced structures (PBSs) were identified in the solar wind, but their formation mechanism remains unclear. This work aims to reveal the dependence of the properties of small-scale PBSs on the background magnetic field (B 0) direction and thus to corroborate the in situ mechanism that forms them. We analyze the plasma and magnetic field data obtained by WIND in the quiet solar wind at 1 AU. First, we use a developed moving-average method to obtain B 0(s, t) for every temporal scale (s) at each time moment (t). By wavelet cross-coherence analysis, we obtain the correlation coefficients between the thermal pressure P th and the magnetic pressure P B, distributing against the temporal scale and the angle θxB between B 0(s, t) and Geocentric Solar Ecliptic coordinates (GSE)-x. We note that the angle coverage of a PBS decreases with shorter temporal scale, but the occurrence of the PBSs is independent of θxB. Suspecting that the isolated small PBSs are formed by compressive waves in situ, we continue this study by testing the wave modes forming a small-scale PBS with B 0(s, t) quasi-parallel to GSE-x. As a result, we identify that the cross-helicity and the compressibility attain values for a slow mode from theoretical calculations. The wave vector is derived from minimum variance analysis. Besides, the proton temperatures obey T < T ∥ derived from the velocity distribution functions, excluding a mirror mode, which is the other candidate for the formation of PBSs in situ. Thus, a small-scale PBS is shown to be driven by oblique, slow-mode waves in the solar wind.

In situ gasification process for producing product gas enriched in carbon monoxide and hydrogen

DOEpatents

Capp, John P.; Bissett, Larry A.

1978-01-01

The present invention is directed to an in situ coal gasification process wherein the combustion zone within the underground coal bed is fed with air at increasing pressure to increase pressure and temperature in the combustion zone for forcing product gases and water naturally present in the coal bed into the coal bed surrounding the combustion zone. No outflow of combustion products occurs during the build-up of pressure and temperature in the combustion zone. After the coal bed reaches a temperature of about 2000.degree. F and a pressure in the range of about 100-200 psi above pore pressure the airflow is terminated and the outflow of the combustion products from the combustion zone is initiated. The CO.sub.2 containing gaseous products and the water bleed back into the combustion zone to react endothermically with the hot carbon of the combustion zone to produce a burnable gas with a relatively high hydrogen and carbon monoxide content. About 11 to 29 percent of the gas recovered from the combustion zone is carbon monoxide which is considerably better than the 4 to 10 percent carbon monoxide obtained by employing previously known coal gasification techniques.

New insights into the mechanism of interaction between CO2 and polymers from thermodynamic parameters obtained by in situ ATR-FTIR spectroscopy.

PubMed

Gabrienko, Anton A; Ewing, Andrew V; Chibiryaev, Andrey M; Agafontsev, Alexander M; Dubkov, Konstantin A; Kazarian, Sergei G

2016-03-07

This work reports new physical insights of the thermodynamic parameters and mechanisms of possible interactions occurring in polymers subjected to high-pressure CO2. ATR-FTIR spectroscopy has been used in situ to determine the thermodynamic parameters of the intermolecular interactions between CO2 and different functional groups of the polymers capable of specific interactions with sorbed CO2 molecules. Based on the measured ATR-FTIR spectra of the polymer samples subjected to high-pressure CO2 (30 bar) at different temperatures (300-340 K), it was possible to characterize polymer-polymer and CO2-polymer interactions. Particularly, the enthalpy and entropy of the formation of the specific non-covalent complexes between CO2 and the hydroxy (-OH), carbonyl (C[double bond, length as m-dash]O) and hydroxyimino ([double bond, length as m-dash]N-OH) functional groups of the polymer samples have been measured. Furthermore, the obtained spectroscopic results have provided an opportunity for the structure of these complexes to be proposed. An interesting phenomenon regarding the behavior of CO2/polymer systems has also been observed. It has been found that only for the polyketone, the value of enthalpy was negative indicating an exothermic process during the formation of the CO2-polymer non-covalent complexes. Conversely, for the polyoxime and polyalcohol samples there is a positive enthalpy determined. This is a result of the initial polymer-polymer interactions requiring more energy to break than is released during the formation of the CO2-polymer complex. The effect of increasing temperature to facilitate the breaking of the polymer-polymer interactions has also been observed. Hence, a mechanism for the formation of CO2-polymer complexes was suggested based on these results, which occurs via a two-step process: (1) the breaking of the existing polymer-polymer interactions followed by (2) the formation of new CO2-polymer non-covalent interactions.

Quantitative depth profiling of Ce(3+) in Pt/CeO2 by in situ high-energy XPS in a hydrogen atmosphere.

PubMed

Kato, Shunsuke; Ammann, Markus; Huthwelker, Thomas; Paun, Cristina; Lampimäki, Markus; Lee, Ming-Tao; Rothensteiner, Matthäus; van Bokhoven, Jeroen A

2015-02-21

The redox property of ceria is a key factor in the catalytic activity of ceria-based catalysts. The oxidation state of well-defined ceria nanocubes in gas environments was analysed in situ by a novel combination of near-ambient pressure X-ray Photoelectron Spectroscopy (XPS) and high-energy XPS at a synchrotron X-ray source. In situ high-energy XPS is a promising new tool to determine the electronic structure of matter under defined conditions. The aim was to quantitatively determine the degree of cerium reduction in a nano-structured ceria-supported platinum catalyst as a function of the gas environment. To obtain a non-destructive depth profile at near-ambient pressure, in situ high-energy XPS analysis was performed by varying the kinetic energy of photoelectrons from 1 to 5 keV, and, thus, the probing depth. In ceria nanocubes doped with platinum, oxygen vacancies formed only in the uppermost layers of ceria in an atmosphere of 1 mbar hydrogen and 403 K. For pristine ceria nanocubes, no change in the cerium oxidation state in various hydrogen or oxygen atmospheres was observed as a function of probing depth. In the absence of platinum, hydrogen does not dissociate and, thus, does not lead to reduction of ceria.

In Situ Atmospheric Pressure Measurements in the Martian Southern Polar Region: Mars Volatiles and Climate Surveyor Meteorology Package on the Mars Polar Lander

NASA Technical Reports Server (NTRS)

Harri, A.-M.; Polkko, J.; Siili, T.; Crisp, D.

1998-01-01

Pressure observations are crucial for the success of the Mars Volatiles and Climate Surveyor (MVACS) Meteorology (MET) package onboard the Mars Polar Lander (MPL), due for launch early next year. The spacecraft is expected to land in December 1999 (L(sub s) = 256 degrees) at a high southern latitude (74 degrees - 78 degrees S). The nominal period of operation is 90 sols but may last up to 210 sols. The MVACS/MET experiment will provide the first in situ observations of atmospheric pressure, temperature, wind, and humidity in the southern hemisphere of Mars and in the polar regions. The martian atmosphere goes through a large-scale atmospheric pressure cycle due to the annual condensation/sublimation of the atmospheric CO2. Pressure also exhibits short period variations associated with dust storms, tides, and other atmospheric events. A series of pressure measurements can hence provide us with information on the large-scale state and dynamics of the atmosphere, including the CO2 and dust cycles as well as local weather phenomena. The measurements can also shed light on the shorter time scale phenomena (e.g., passage of dust devils) and hence be important in contributing to our understanding of mixing and transport of heat, dust, and water vapor.

A revised and unified pressure-clamp/relaxation theory for studying plant cell water relations with pressure probes: in-situ determination of cell volume for calculation of volumetric elastic modulus and hydraulic conductivity.

PubMed

Knipfer, T; Fei, J; Gambetta, G A; Shackel, K A; Matthews, M A

2014-10-21

The cell-pressure-probe is a unique tool to study plant water relations in-situ. Inaccuracy in the estimation of cell volume (νo) is the major source of error in the calculation of both cell volumetric elastic modulus (ε) and cell hydraulic conductivity (Lp). Estimates of νo and Lp can be obtained with the pressure-clamp (PC) and pressure-relaxation (PR) methods. In theory, both methods should result in comparable νo and Lp estimates, but this has not been the case. In this study, the existing νo-theories for PC and PR methods were reviewed and clarified. A revised νo-theory was developed that is equally valid for the PC and PR methods. The revised theory was used to determine νo for two extreme scenarios of solute mixing between the experimental cell and sap in the pressure probe microcapillary. Using a fully automated cell-pressure-probe (ACPP) on leaf epidermal cells of Tradescantia virginiana, the validity of the revised theory was tested with experimental data. Calculated νo values from both methods were in the range of optically determined νo (=1.1-5.0nL) for T. virginiana. However, the PC method produced a systematically lower (21%) calculated νo compared to the PR method. Effects of solute mixing could only explain a potential error in calculated νo of <3%. For both methods, this discrepancy in νo was almost identical to the discrepancy in the measured ratio of ΔV/ΔP (total change in microcapillary sap volume versus corresponding change in cell turgor) of 19%, which is a fundamental parameter in calculating νo. It followed from the revised theory that the ratio of ΔV/ΔP was inversely related to the solute reflection coefficient. This highlighted that treating the experimental cell as an ideal osmometer in both methods is potentially not correct. Effects of non-ideal osmotic behavior by transmembrane solute movement may be minimized in the PR as compared to the PC method. Copyright © 2014 Elsevier Ltd. All rights reserved.

Melting of KCl and pressure calibration from in situ ionic conductivity measurements in a multi-anvil apparatus

NASA Astrophysics Data System (ADS)

Li, J.; Dong, J.; Zhu, F.

2017-12-01

Melting plays an unparalleled role in planetary differentiation processes including the formation of metallic cores, basaltic crusts, and atmospheres. Knowledge of the melting behavior of Earth materials provides critical constraints for establishing the Earth's thermal structure, interpreting regional seismic anomalies, and understanding the nature of chemical heterogeneity. Measuring the melting points of compressed materials, however, have remained challenging mainly because melts are often mobile and reactive, and temperature and pressure gradients across millimeter or micron-sized samples introduce large uncertainties in melting detection. Here the melting curve of KCl was determined through in situ ionic conductivity measurements, using the multi-anvil apparatus at the University of Michigan. The method improves upon the symmetric configuration that was used recently for studying the melting behaviors of NaCl, Na2CO3, and CaCO3 (Li and Li 2015 American Mineralogist, Li et al. 2017 Earth and Planetary Science Letters). In the new configuration, the thermocouple and electrodes are placed together with the sample at the center of a cylindrical heater where the temperature is the highest along the axis, in order to minimize uncertainties in temperature measurements and increase the stability of the sample and electrodes. With 1% reproducibility in melting point determination at pressures up to 20 GPa, this method allows us to determine the sample pressure to oil load relationship at high temperatures during multiple heating and cooling cycles, on the basis of the well-known melting curves of ionic compounds. This approach enables more reliable pressure measurements than relying on a small number of fixed-point phase transitions. The new data on KCl bridge the gap between the piston-cylinder results up to 4 GPa (Pistorius 1965 J. of Physics and Chemistry of Solids) and several diamond-anvil cell data points above 20 GPa (Boehler et al. 1996 Physical Review). We

In Situ High Temperature High Pressure MAS NMR Study on the Crystallization of AlPO 4 -5

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

Zhao, Zhenchao; Xu, Suochang; Hu, Mary Y.

2016-01-28

A damped oscillating crystallization process of AlPO4-5 at the presence of small amount of water is demonstrated by in situ high temperature high pressure multinuclear MAS NMR. Crystalline AlPO4-5 is formed from an intermediate semicrystalline phase via continuous rearrangement of the local structure of amorphous precursor gel. Activated water catalyzes the rearrangement via repeatedly hydrolysis and condensation reaction. Strong interactions between organic template and inorganic species facilitate the ordered rearrangement. During the crystallization process, excess water, phosphate, and aluminums are expelled from the precursor. The oscillating crystallization reflects mass transportation between the solid and liquid phase during the crystallization process.more » This crystallization process is also applicable to AlPO4-5 crystallized in the presence of a relatively large amount of water.« less

In Situ Measurement of Ground-Surface Flow Resistivity

NASA Technical Reports Server (NTRS)

Zuckerwar, A. J.

1984-01-01

New instrument allows in situ measurement of flow resistivity on Earth's ground surface. Nonintrusive instrument includes specimen holder inserted into ground. Flow resistivity measured by monitoring compressed air passing through flow-meters; pressure gages record pressure at ground surface. Specimen holder with knife-edged inner and outer cylinders easily driven into ground. Air-stream used in measuring flow resistivity of ground enters through quick-connect fitting and exits through screen and venthole.

In situ study of mass transfer in aqueous solutions under high pressures via Raman spectroscopy: A new method for the determination of diffusion coefficients of methane in water near hydrate formation conditions

USGS Publications Warehouse

Lu, W.J.; Chou, I.-Ming; Burruss, R.C.; Yang, M.Z.

2006-01-01

A new method was developed for in situ study of the diffusive transfer of methane in aqueous solution under high pressures near hydrate formation conditions within an optical capillary cell. Time-dependent Raman spectra of the solution at several different spots along the one-dimensional diffusion path were collected and thus the varying composition profile of the solution was monitored. Diffusion coefficients were estimated by the least squares method based on the variations in methane concentration data in space and time in the cell. The measured diffusion coefficients of methane in water at the liquid (L)-vapor (V) stable region and L-V metastable region are close to previously reported values determined at lower pressure and similar temperature. This in situ monitoring method was demonstrated to be suitable for the study of mass transfer in aqueous solution under high pressure and at various temperature conditions and will be applied to the study of nucleation and dissolution kinetics of methane hydrate in a hydrate-water system where the interaction of methane and water would be more complicated than that presented here for the L-V metastable condition. ?? 2006 Society for Applied Spectroscopy.

New structural phase obtained by exerting high pressure on (Br2)n@AFI composite material

NASA Astrophysics Data System (ADS)

Yao, Zhen; Lv, Jia-Yin; Liu, Bo; Liu, Bing-Bing; Yang, Bai

2018-06-01

In this paper, we present a theoretical study on the high-pressure behaviors of a (Br2)n@AlPO4-5 (AFI) peapod structure. The influence of the encapsulated Br2 molecule on the structural deformation of AFI crystal is analyzed using the volume-pressure function. The bonding process of the linearly arrayed Br2 molecule transferring to the bromine atomic chain is analyzed by the electron density distribution. A new high-pressure phase with P2 point group symmetry is obtained as the pressure increases to 34 GPa. In addition, electron density difference calculations are used to study the systematic charge transformation. Further analysis indicates that the encapsulated Br2 molecules can significantly modify the electronic structure of the AFI crystal. The band gap of the (Br2)n@AFI decreases with pressure and closes at 9 GPa. Moreover, the calculated bulk modulus and electronic properties indicate that the new structural phase is metallic with a high hardness, providing a new strategy for exploring novel nanomaterials.

In Situ Monitoring of Particle Consolidation During Low Pressure Cold Spray by Ultrasonic Techniques

NASA Astrophysics Data System (ADS)

Maev, R. Gr.; Titov, S.; Leshchynsky, V.; Dzhurinskiy, D.; Lubrick, M.

2011-06-01

This study attempts to test the viability of the examination of the cold spray process using acoustic methods, specifically in situ testing during the actual spray process itself. Multiple composites studied by flat and multi-channel transducers as well as the results of actual online measurements are presented. It is shown that the final thickness as well as the dynamics of buildup can be evaluated (including plotting rates of buildup). Cross sections of the coating thickness are also easy to obtain and show true profiles of the coating. The data can also be used to generate real estimates for nozzle speed and spray diameter. Finally, comparisons of real thickness and acoustically estimated thickness show a close linear relationship. The data clearly show that online acoustic measurement is a viable method for estimating thickness buildup.

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.

Identifying mechanical property parameters of planetary soil using in-situ data obtained from exploration rovers

NASA Astrophysics Data System (ADS)

Ding, Liang; Gao, Haibo; Liu, Zhen; Deng, Zongquan; Liu, Guangjun

2015-12-01

Identifying the mechanical property parameters of planetary soil based on terramechanics models using in-situ data obtained from autonomous planetary exploration rovers is both an important scientific goal and essential for control strategy optimization and high-fidelity simulations of rovers. However, identifying all the terrain parameters is a challenging task because of the nonlinear and coupling nature of the involved functions. Three parameter identification methods are presented in this paper to serve different purposes based on an improved terramechanics model that takes into account the effects of slip, wheel lugs, etc. Parameter sensitivity and coupling of the equations are analyzed, and the parameters are grouped according to their sensitivity to the normal force, resistance moment and drawbar pull. An iterative identification method using the original integral model is developed first. In order to realize real-time identification, the model is then simplified by linearizing the normal and shearing stresses to derive decoupled closed-form analytical equations. Each equation contains one or two groups of soil parameters, making step-by-step identification of all the unknowns feasible. Experiments were performed using six different types of single-wheels as well as a four-wheeled rover moving on planetary soil simulant. All the unknown model parameters were identified using the measured data and compared with the values obtained by conventional experiments. It is verified that the proposed iterative identification method provides improved accuracy, making it suitable for scientific studies of soil properties, whereas the step-by-step identification methods based on simplified models require less calculation time, making them more suitable for real-time applications. The models have less than 10% margin of error comparing with the measured results when predicting the interaction forces and moments using the corresponding identified parameters.

Nanocapsule of cationic liposomes obtained using "in situ" acrylic acid polymerization: stability, surface charge and biocompatibility.

PubMed

Scarioti, Giovana Danieli; Lubambo, Adriana; Feitosa, Judith P A; Sierakowski, Maria Rita; Bresolin, Tania M B; de Freitas, Rilton Alves

2011-10-15

In this work, didecyldimethylammonium bromide (DDAB) and 1,2-dioleoyl-sn-glycero-3-phosphatidylethanolamine (DOPE) (2.5:1) were used to prepare liposomes coated with polyacrylic acid (PAA) using "in situ" polymerization with 2.5, 5 and 25 mM of acrylic acid (AA). The PAA concentrations were chosen to achieve partially to fully covered capsules, and the polymerization reaction was observed with real-time monitoring using dynamic light scattering (NanoDLS). The DDAB:DOPE liposomes showed stability in the tested temperature range (25-70°C), whereas the results confirmed the success of the polymerization according to superficial charge (zeta potential of +66.7±1.2 mV) results and AFM images. For the liposomes that were fully coated with PAA (zeta potential of +0.3±3.9 mV), cytotoxicity was independent of the concentration of albumin. Cationic liposomes and nanocapsules of the stable liposomes coated with PAA were obtained by controlling the surface charge, which was the most important factor related to cytotoxicity. Thus, a potential, safe drug nanocarrier was successfully developed in this work. Copyright © 2011 Elsevier B.V. All rights reserved.

Digestive efficiencies of ex situ and in situ West Indian manatees (Trichechus manatus latirostris).

PubMed

Worthy, Graham A J; Worthy, Tamara A M

2014-01-01

Digestive efficiencies (Dm) of ex situ and in situ manatees (Trichechus manatus latirostris) were, for the first time, assessed using manganese (Mn(2+)) as a naturally occurring marker. The Dm of ex situ manatees determined using [Mn(2+)] did not differ significantly from the Dm assessed using lignin, supporting the efficacy of the manganese approach. Gastrointestinal tract samples, obtained from recently dead animals, showed [Mn(2+)] concentrations were lowest in the stomach and remained low in the duodenum and small intestine but increased in the cecum, colon, and rectum, consistent with colonic digestion and absorption. In situ manatees consuming marine vegetation had significantly lower Dm (mean ± SE, 46.9% ± 1.8%; n=8) than did in situ manatees consuming freshwater vegetation (77.8% ± 2.6%; n=7), which in turn had significantly lower values than did ex situ manatees consuming lettuce (84.0% ± 0.7%; n=37). In situ manatees eating seagrasses had significantly higher Dm than did long-term ex situ animals consuming seagrass for short periods of time (46.9% ± 1.8% vs. 36.2% ± 1.2%, respectively), suggesting potential modification of gut flora over time. One significant ramification of our results is that manatees consuming seagrasses would require a greater standing biomass to support their needs than would be required if they were eating freshwater vegetation. This reinforces the critical need to implement habitat conservation and protection before considering downlisting or delisting manatees as an endangered species.

In Situ Density Measurement of Basaltic Melts at High Pressure by X-ray Absorption Method

NASA Astrophysics Data System (ADS)

Ando, R.; Ohtani, E.; Suzuki, A.; Urakawa, S.; Katayama, Y.

2004-12-01

Density of silicate melt at high pressure is one of the most important properties to understand magma migration in the planetary interior. However, because of experimental difficulties, the density of magma at high pressure is poorly known. Katayama et al. (1996) recently developed a new in situ density measurement method for metallic melts, based on the density dependency of X-ray absorption in the sample. In this study, we tried to measure the density of basaltic melt by this absorption method. When X-ray is transmitted to the sample, the intensity of the transmitted X-ray beam (I) is expressed as follows; I=I0exp(-μ ρ t), where I0 is the intensity of incident X-ray beam, μ is the mass absorption coefficient, ρ is the density of the sample, and t is the thickness of the sample. If t and μ are known, we can determine the density of the sample by measuring I and I0. This is the principle of the absorption method for density measurement. In this study, in order to determine t, we used a single crystalline diamond cylinder as a sample capsule, diamond is less compressive and less deformable so that even at high pressure t (thickness of the sample at the point x) is expressed as follows; t = 2*(R02-x2)1/2, R0 is the inner radius of cylinder at the ambient condition, and x is distance from a center of the capsule. And diamond also shows less absorption so that this make it possible to measure the density of silicate melt with smaller absorption coefficient than metallic melts. In order to know the μ of the sample, we measured both densities (ρ ) and absorptions (I/I0) for some glasses and crystals with same composition of the sample at the ambient condition, and calculated as fallows; μ =ln(I/I0)/ρ . Experiments were made at the beamline (BL22XU) of SPring-8. For generation of high pressure and high temperature, we used DIA-type cubic anvil apparatus (SMAP180) there. We used tungsten carbide anvils with the edge-length of 6 mm. The energy of monochromatic X

Uranium oxidation kinetics monitored by in-situ X-ray diffraction

NASA Astrophysics Data System (ADS)

Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-01

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

Enhanced structural stability and photo responsiveness of CH 3NH 3SnI 3 perovskite via pressure-induced amorphization and recrystallization

DOE PAGES

Lu, Xujie; Wang, Yonggang; Stoumpos, Constantinos C.; ...

2016-10-01

An organic–inorganic halide CH 3NH 3SnI 3 perovskite with significantly improved structural stability is obtained via pressure-induced amorphization and recrystallization. In situ high-pressure resistance measurements reveal an increased electrical conductivity by 300% in the pressure-treated perovskite. Photocurrent measurements also reveal a substantial enhancement in visible-light responsiveness. In conclusion, the mechanism underlying the enhanced properties is shown to be associated with the pressure-induced structural modification.

In situ x-ray diffraction observation of multiple texture turnovers in sputtered Cr films

NASA Astrophysics Data System (ADS)

Zhao, Z. B.; Rek, Z. U.; Yalisove, S. M.; Bilello, J. C.

2004-11-01

A series of Cr films were deposited onto native oxides of (100) Si substrates via a confocal deposition geometry in a magnetron sputter chamber. The film growth chamber was incorporated with an in situ x-ray diffraction system, which allowed the collection of x-ray diffraction data on the growing film in a quasi real time fashion without interruption of film deposition. The in situ x-ray diffraction, coupled with other ex situ characterization techniques, was used to study structural evolutions of the Cr films deposited at various Ar pressures. It was observed that the evolution of the crystallographic structures of Cr films was very sensitive to both deposition conditions and film thickness. With the confocal deposition geometry, the Cr films developed various types of out-of-plane textures. In addition to the (110) and (100) types of textures commonly reported for vapor deposited Cr films, the (111) and (112) types of textures were also observed. The film deposited at low Ar pressure (2 mTorr) developed strong (111) type texture. With the increase in either Ar pressure or film thickness, the Cr films tended to develop (112) and (100) types of texture. At high Ar pressures (>10 mTorr), several changes in texture type with increasing film thickness were observed. The sequence can be described as (110)-->(112)-->(100). The strong tendency for these films to ultimately assume the (100) type of texture could be related to significant rises in substrate temperatures during the late stages of film growth with high Ar pressures. The observation of the multiple texture type changes suggests that the evolution of Cr films is controlled by complex growth kinetics. The competitive growth of grains with different orientations can be altered not only by controllable deposition parameters such as Ar pressure, but also by the variations of in situ film attributes (e.g., residual stress and substrate temperature) occurring concurrently with film growth.

In situ electrostatic characterisation of ion beams in the region of ion acceleration

NASA Astrophysics Data System (ADS)

Bennet, Alexander; Charles, Christine; Boswell, Rod

2018-02-01

In situ and ex situ techniques have been used to measure directional ion beams created by a sharp axial potential drop in low pressure expanding plasmas. Although Retarding Field Energy Analysers (RFEAs) are the most convenient technique to measure the ion velocities and plasma potentials along with the plasma density, they are bulky and are contained in a grounded shield that may perturb the electric potential profile of the expanding plasma. In principle, ex situ techniques produce a more reliable measurement and Laser Induced Fluorescence spectroscopy (LIF) has previously been used to characterise the spatial velocity profile of ion beams in the same region of acceleration for a range of pressures. Here, satisfactory agreement between the ion velocity profiles measured by LIF and RFEA techniques has allowed the RFEA method to be confidently used to probe the ion beam characteristics in the regions of high gradients in plasma density and DC electric fields which have previously proven difficult.

In situ 3D-X-ray diffraction tracking of individual grains of olivine during high-pressure/ high-temperature phase transitions

NASA Astrophysics Data System (ADS)

Rosa, A. D.; Merkel, S.; Ghosh, S.; Hilairet, N.; Perrillat, J.; Mezouar, N.; Vaughan, G.

2013-12-01

The series of phase transitions between olivine, wadsleyite and ringwoodite play an essential role for large scale dynamical processes in the Earth mantle. Detailed knowledge of the microscopic mechanism at the origin of these high-pressure and high-temperature phase transformations is useful to connect global seismic observations and geodynamics. Indeed, the textures of these phases can be induced either during mantle flow or during the phase transformations and they greatly affect the characteristics of seismic wave propagation. Here, we present a new design of diamond anvil cell experiments to collect three-dimensional diffraction images and track individual grains inside a polycristalline sample at high pressure and high temperature. The instrumentation includes a new resistively heated diamond anvil cell developed at beamline ID27 of the ESRF which provided stable and homogenous temperature condition over more than 24 hours. In our experiments, the pressure is first increased up to 12 GPa at a constant temperature of T = 800 K. The temperature is then further increased to 1300 K to reach the stability field of the high-pressure polymorph. Upon further compression the transformation of olivine to its high-pressure polymorph is successfully monitored. At each pressure-temperature step and while the sample is transforming the crystallographic parameters, the orientations and positions of grains within the sample are tracked in situ using three-dimensional X-ray diffraction. This will provide important information on the micromechanical properties of olivine including orientation statistics, orientation relations between parent and daughter phases, and transformation textures at different stages of the phase transition. This in turn will help in interpreting the geophysical observations. Details of the experimental and analytical approach used in this study will be given.

Estimation of In Situ Stress and Permeability from an Extended Leak-off Test

NASA Astrophysics Data System (ADS)

Nghiep Quach, Quoc; Jo, Yeonguk; Chang, Chandong; Song, Insun

2016-04-01

Among many parameters needed to analyze a variety of geomechanical problems related to subsurface CO2 storage projects, two important ones are in situ stress states and permeability of the storage reservoirs and cap rocks. In situ stress is needed for investigating potential risk of fault slip in the reservoir systems and permeability is needed for assessing reservoir flow characteristics and sealing capability of cap rocks. We used an extended leak-off test (XLOT), which is often routinely conducted to assess borehole/casing integrity as well as fracture gradient, to estimate both in situ least principal stress magnitude and in situ permeability in a CO2 storage test site, offshore southeast Korea. The XLOT was conducted at a casing shoe depth (700 m below seafloor) within the cap rock consisting of mudstone, approximately 50 m above the interface between cap rock and storage reservoir. The test depth was cement-grouted and remained for 4 days for curing. Then the hole was further drilled below the casing shoe to create a 4 m open-hole interval at the bottom. Water was injected using hydraulic pump at an approximately constant flowrate into the bottom interval through the casing, during which pressure and flowrate were recorded continuously at the surface. The interval pressure (P) was increased linearly with time (t) as water was injected. At some point, the slope of P-t curve deviated from the linear trend, which indicates leak-off. Pressure reached its peak upon formation breakdown, followed by a gradual pressure decrease. Soon after the formation breakdown, the hole was shut-in by pump shut-off, from which we determined the instantaneous shut-in pressure (ISIP). The ISIP was taken to be the magnitude of the in situ least principal stress (S3), which was determined to be 12.1 MPa. This value is lower than the lithostatic vertical stress, indicating that the S3 is the least horizontal principal stress. The determined S3 magnitude will be used to characterize the

Pressure induced para-antiferromagnetic switching in BiFeO3-PbTiO3 as determined using in-situ neutron diffraction

NASA Astrophysics Data System (ADS)

Comyn, Tim P.; Stevenson, Tim; Al-Jawad, Maisoon; Marshall, William G.; Smith, Ronald I.; Herrero-Albillos, Julia; Cywinski, Robert; Bell, Andrew J.

2013-05-01

BiFeO3-PbTiO3 exhibits both ferroelectric and antiferromagnetic order, depending on the composition. Moderate hydrostatic pressures have been used at room temperature to transform the crystallographic phase from P4mm to R3c for the compositions 0.7BiFeO3-0.3PbTiO3 and 0.65BiFeO3-0.35PbTiO3, as determined using in-situ neutron diffraction. Using Rietveld refinements, the resultant data showed that, for both compositions, a transformation from para- to G-type antiferromagnetic order accompanied the structural transition. The transformation occurred over the range 0.4-0.77 and 0.67-0.88 GPa for 0.7BiFeO3-0.3PbTiO3 and 0.65BiFeO3-0.35PbTiO3, respectively; at intermediate pressures, a mixture of P4mm and R3c phases were evident. These pressures are far lower than required to induce a phase transition in either the BiFeO3 or PbTiO3 end members. The driving force for this pressure induced first order phase transition is a significant difference in volume between the two phases, P4mm > R3c of 4%-5%, at ambient pressure. Upon removal of the pressure, 0.65BiFeO3-0.35PbTiO3 returned to the paramagnetic tetragonal state, whereas in 0.7BiFeO3-0.3PbTiO3 antiferromagnetic ordering persisted, and the structural phase remained rhombohedral. Using conventional laboratory x-ray diffraction with a hot-stage, the phase readily reverted back to a tetragonal phase, at temperatures between 100 and 310 °C for 0.7BiFeO3-0.3PbTiO3, far lower than the ferroelectric Curie point for this composition of 632 °C. To our knowledge, the reported pressure induced para- to antiferromagnetic transition is unique in the literature.

Raman scattering from superhard rhenium diboride under high pressure

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

Xie, Miao; Winkler, Björn; Mao, Zhu

2014-01-06

Lattice vibrational properties of superhard rhenium diboride (ReB{sub 2}) were examined up to 8 GPa in a diamond anvil cell using Raman spectroscopy techniques. Linear pressure coefficients and mode Grüneisen parameters are obtained. Good agreement is found between the experimental and theoretical calculated Grüneisen parameters. Examination of the calculated mode Grüneisen parameters reveals that both B-B and Re-B covalent bonds play a dominant role in supporting the applied load under pressure. A comparison of vibrations parallel and perpendicular to the c-axis indicates that bonds along the c-axis tend to take greater loads. Our results agree with observations of elastic lattice anisotropymore » obtained from both in situ X-ray diffraction measurements and ultrasonic resonance spectra.« less

In-situ stresses in low-permeability, nonmarine rocks

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

Warpinski, N.R.; Teufel, L.W.

In-situ stress measurements have been performed over a 2,500-ft (760-m) interval in the nonmarine section of the Cretaceous Mesaverde in the Piceance basin in Colorado. These measurements included 52 hydraulic fracture measurements of the minimum in-situ stress and 22 anelastic strain recovery (ASR) measurements. Stress data obtained in sandstones, shales, mudstones, siltstones, and coals show the effect of lithology on the magnitudes of the stresses.

A high-pressure atomic force microscope for imaging in supercritical carbon dioxide

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

Lea, Alan S.; Higgins, Steven R.; Knauss, Kevin G.

2011-04-26

A high-pressure atomic force microscope (AFM) that enables in-situ, atomic scale measurements of topography of solid surfaces in contact with supercritical CO2 (scCO2) fluids has been developed. This apparatus overcomes the pressure limitations of the hydrothermal AFM and is designed to handle pressures up to 100 atm at temperatures up to ~ 350 K. A standard optically-based cantilever deflection detection system was chosen. When imaging in compressible supercritical fluids such as scCO2, precise control of pressure and temperature in the fluid cell is the primary technical challenge. Noise levels and imaging resolution depend on minimization of fluid density fluctuations thatmore » change the fluid refractive index and hence the laser path. We demonstrate with our apparatus in-situ atomic scale imaging of a calcite (CaCO3) mineral surface in scCO2; both single, monatomic steps and dynamic processes occurring on the (10¯14) surface are presented. This new AFM provides unprecedented in-situ access to interfacial phenomena at solid-fluid interfaces under pressure.« less

In situ measurement of velocity-stress sensitivity using crosswell continuous active-source seismic monitoring

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

Marchesini, P; Ajo-Franklin, JB; Daley, TM

2017-09-01

© 2017 Society of Exploration Geophysicists. The ability to characterize time-varying reservoir properties, such as the state of stress, has fundamental implications in subsurface engineering, relevant to geologic sequestration of CO2. Stress variation, here in the form of changes in pore fluid pressure, is one factor known to affect seismic velocity. Induced variations in velocity have been used in seismic studies to determine and monitor changes in the stress state. Previous studies conducted to determine velocity-stress sensitivity at reservoir conditions rely primarily on laboratory measurements of core samples or theoretical relationships. We have developed a novel field-scale experiment designed tomore » study the in situ relationship between pore-fluid pressure and seismic velocity using a crosswell continuous active-source seismic monitoring (CASSM) system. At the Cranfield, Mississippi, CO2 sequestration field site, we actively monitored seismic response for five days with a temporal resolution of 5 min; the target was a 26 m thick injection zone at approximately 3.2 km depth in a fluvial sandstone formation (lower Tuscaloosa Formation). The variation of pore fluid pressure was obtained during discrete events of fluid withdrawal from one of the two wells and monitored with downhole pressure sensors. The results indicate a correlation between decreasing CASSM time delay (i.e., velocity change for a raypath in the reservoir) and periods of reduced fluid pore pressure. The correlation is interpreted as the velocity-stress sensitivity measured in the reservoir. This observation is consistent with published laboratory studies documenting a velocity (V) increase with an effective stress increase. A traveltime change (dt) of 0.036 ms is measured as the consequence of a change in pressure of approximately 2.55 MPa (dPe). For T 1/4 13 ms total traveltime, the velocity-stress sensitivity is dV/V/dPe 1/4 dt/T/dPe 1/4 10.9 × 10-4/MPa. The overall results suggest

Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

PubMed

Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

2013-10-01

In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

In situ study of an oxidation reaction on a Pt/C electrode by ambient pressure hard X-ray photoelectron spectroscopy

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

Takagi, Yasumasa, E-mail: ytakagi@ims.ac.jp; Uemura, Yohei; Yokoyama, Toshihiko

2014-09-29

We have constructed an ambient pressure X-ray photoelectron spectroscopy instrument that uses hard X-ray radiation at the high-performance undulator beamline BL36XU of SPring-8. The dependence of the Au 4f peak intensity from Au foil on the ambient N{sub 2} pressure was measured. At a photon energy of 7.94 keV, the Au 4f peak intensity maintained 40% at 3000 Pa compared with that at high vacuum. We designed a polymer electrolyte fuel cell that allows us to perform X-ray photoelectron spectroscopy measurements of an electrode under working conditions. The oxidized Pt peaks were observed in the Pt 3d{sub 5/2} level of Pt nanoparticlesmore » in the cathode, and the peaks clearly depended on the applied voltage between the anode and cathode. Our apparatus can be applied as a valuable in situ tool for the investigation of the electronic states and adsorbed species of polymer electrolyte fuel cell electrode catalysts under the reaction conditions.« 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

Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions

NASA Astrophysics Data System (ADS)

Richard, M.-I.; Fernández, S.; Hofmann, J. P.; Gao, L.; Chahine, G. A.; Leake, S. J.; Djazouli, H.; De Bortoli, Y.; Petit, L.; Boesecke, P.; Labat, S.; Hensen, E. J. M.; Thomas, O.; Schülli, T.

2017-09-01

A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10-2-103 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

In situ investigation of supercritical CO2 assisted impregnation of drugs into a polymer by high pressure FTIR micro-spectroscopy.

PubMed

Champeau, M; Thomassin, J-M; Jérôme, C; Tassaing, T

2015-02-07

An original experimental set-up combining a FTIR micro-spectrometer with a high pressure cell has been built in order to analyze in situ the impregnation of a solute into microscopic polymer samples, such as fibers or films, subjected to supercritical CO2. Thanks to this experimental set-up, key factors governing the impregnation process can be simultaneously followed such as the swelling of the polymeric matrix, the CO2 sorption, the kinetics of impregnation and the drug loading into the matrix. Moreover, the solute/polymer interactions and the speciation of the solute can be analyzed. We have monitored in situ the impregnation of aspirin and ketoprofen into PEO (Polyethylene Oxide) platelets at T = 40 °C and P = 5; 10 and 15 MPa. The kinetics of impregnation of aspirin was quicker than the one of ketoprofen and the final drug loading was also higher in the case of aspirin. Whereas the CO2 sorption and the PEO swelling remain constant when PEO is just subjected to CO2 under isobaric conditions, we noticed that both parameters can increase while the drug impregnates PEO. Coupling these results with DSC measurements, we underlined the plasticizing effect of the drug that also leads to a decrease in the crystallinity of PEO in situ thus favoring the sorption of CO2 molecules into the matrix and the swelling of the matrix. The plasticizing effect increases with the drug loading. Finally, the speciation of drugs was investigated considering the shift of the carboxyl bands of the drugs. Both drugs were found to be mainly homogeneously dispersed into PEO.

Multipurpose high-pressure high-temperature diamond-anvil cell with a novel high-precision guiding system and a dual-mode pressurization device

NASA Astrophysics Data System (ADS)

Pippinger, Thomas; Miletich, Ronald; Burchard, Michael

2011-09-01

A novel diamond-anvil cell (DAC) design has been constructed and tested for in situ applications at high-pressure (HP) operations and has proved to be suitable even for HP sample environments at non-ambient temperature conditions. The innovative high-precision guiding mechanism, comparable to a dog clutch, consists of perpendicular planar sliding-plane elements and is integrated directly into the base body of the cylindrically shaped DAC. The combination of two force-generating devices, i.e., mechanical screws and an inflatable gas membrane, allows the user to choose independently between, and to apply individually, two different forcing mechanisms for pressure generation. Both mechanisms are basically independent of each other, but can also be operated simultaneously. The modularity of the DAC design allows for an easy exchange of functional core-element groups optimized not only for various analytical in situ methods but also for HP operation with or without high-temperature (HT) application. For HP-HT experiments a liquid cooling circuit inside the specific inner modular groups has been implemented to obtain a controlled and limited heat distribution within the outer DAC body.

High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source†

NASA Astrophysics Data System (ADS)

Toulemonde, Pierre; Goujon, Céline; Laversenne, Laetitia; Bordet, Pierre; Bruyère, Rémy; Legendre, Murielle; Leynaud, Olivier; Prat, Alain; Mezouar, Mohamed

2014-04-01

We have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα 1, 2≈0.56 Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7 mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2.

In situ TEM of radiation effects in complex ceramics.

PubMed

Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

2009-03-01

In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions. (c) 2009 Wiley-Liss, Inc.

IN SITU MAGIC ANGLE SPINNING NMR FOR STUDYING GEOLOGICAL CO(2) SEQUESTRATION

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

Hoyt, David W.; Turcu, Romulus VF; Sears, Jesse A.

2011-03-27

Geological carbon sequestration (GCS) is one of the most promising ways of mitigating atmospheric greenhouse gases (1-3). Mineral carbonation reactions are potentially important to the long-term sealing effectiveness of caprock but remain poorly predictable, particularly in low-water supercritical CO2 (scCO2)-dominated environments where the chemistry has not been adequately explored. In situ probes that provide molecular-level information is desirable for investigating mechanisms and rates of GCS mineral carbonation reactions. MAS-NMR is a powerful tool for obtaining detailed molecular structure and dynamics information of a system regardless whether the system is in a solid, a liquid, a gaseous, or a supercritical state,more » or a mixture thereof (4,5). However, MAS NMR under scCO2 conditions has never been realized due to the tremendous technical difficulties of achieving and maintaining high pressure within a fast spinning MAS rotor (6,7), where non-metal materials must be used. In this work, we report development of a unique high pressure MAS NMR capability, and its application to mineral carbonation chemistry in scCO2 under geologically relevant temperatures and pressures.« less

An ultrahigh vacuum multipurpose specimen chamber with sample introduction system for in situ transmission electron microscopy investigations

NASA Technical Reports Server (NTRS)

Heinemann, K.; Poppa, H.

1986-01-01

A commercial transmission electron microscope (TEM), with flat-plate upper pole piece configuration of the objective lens, and top-entry specimen introduction was modified by introducing an ultrahigh vacuum (UHV) specimen chamber for in situ TEM experimentation. The pumping and design principles and special features of this UHV chamber, which makes it possible to obtain 5 x 10 to the -10th mbar pressure at the site of the specimen, while maintaining the airlock system that allows operation in the 10 to the -10th mbar range within 15 min after specimen change, are described. Design operating pressures and image quality (resolution of metal particles smaller than 1 nm in size) were achieved. Schematic drawings and design dimensions are included.

Development of a new type of high pressure calorimetric cell, mechanically agitated and equipped with a dynamic pressure control system: Application to the characterization of gas hydrates

NASA Astrophysics Data System (ADS)

Plantier, F.; Marlin, L.; Missima, D.; Torré, J.-P.

2013-12-01

A novel prototype of calorimetric cell has been developed allowing experiments under pressure with an in situ agitation system and a dynamic control of the pressure inside the cell. The use of such a system opens a wide range of potential practical applications for determining properties of complex fluids in both pressurized and agitated conditions. The technical details of this prototype and its calibration procedure are described, and an application devoted to the determination of phase equilibrium and phase change enthalpy of gas hydrates is presented. Our results, obtained with a good precision and reproducibility, were found in fairly good agreement with those found in literature, illustrate the various interests to use this novel apparatus.

Enhanced Structural Stability and Photo Responsiveness of CH3 NH3 SnI3 Perovskite via Pressure-Induced Amorphization and Recrystallization.

PubMed

Lü, Xujie; Wang, Yonggang; Stoumpos, Constantinos C; Hu, Qingyang; Guo, Xiaofeng; Chen, Haijie; Yang, Liuxiang; Smith, Jesse S; Yang, Wenge; Zhao, Yusheng; Xu, Hongwu; Kanatzidis, Mercouri G; Jia, Quanxi

2016-10-01

An organic-inorganic halide CH 3 NH 3 SnI 3 perovskite with significantly improved structural stability is obtained via pressure-induced amorphization and recrystallization. In situ high-pressure resistance measurements reveal an increased electrical conductivity by 300% in the pressure-treated perovskite. Photocurrent measurements also reveal a substantial enhancement in visible-light responsiveness. The mechanism underlying the enhanced properties is shown to be associated with the pressure-induced structural modification. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thermodynamics of Silica Dissolution From In-situ Raman +Spectroscopy

NASA Astrophysics Data System (ADS)

Davis, M. K.; Fumagalli, P.; Stixrude, L. P.

2001-12-01

Solubilities of cations, such as silicon, in water strongly effect both the physical and thermodynamical properties of supercritical metamorphic fluids. Modeling the thermodynamics of fluid-rock interactions requires therefore a profound understanding of cation dissolution and aqueous speciation. In-situ Raman experiments of the silica-water system were performed in an externally heated Bassett-type diamond-anvil cell at the Department of Geological Sciences, University of Michigan. Natural quartz samples (from Owl Creek Mountains, Wyoming) were loaded in the sample chamber with de-ionized or spectrographic water. All experiments used doubly polished rhenium gaskets with a thickness of 200 μ m, diameter of 1.0 mm, and a 500 μ m drillhole for the sample chamber. Temperature was measured using K-type thermocouples wrapped around both the upper and lower diamond anvils. Pressures are obtained on the basis of the shift of the 464 cm-1 Raman mode of quartz. In-situ Raman spectra were collected from 250-1200 cm-1, focusing on the vibrational modes of aqueous silica species at temperatures up to 700 ° C and pressures up to 14 kbar. We observed Si-O stretching modes attributable to dimer (H6Si2O7, 965 cm-1) and monomer (H4SiO4, 771 cm-1) aqueous silica species. The relative intensities of these two bands as a function of isochoric heating place constraints on the energetics of the polymerization reaction, if we assume that the intensity ratio is linearly related to concentration ratio. We have been able to perform experiments along two different isochores (0.9 and 0.75 g/cm3, respectively) from which we are able to derive the enthalpy of reaction.

Characterizing spatial and temporal variability of dissolved gases in aquatic environments with in situ mass spectrometry.

PubMed

Camilli, Richard; Duryea, Anthony N

2009-07-01

The TETHYS mass spectrometer is intended for long-term in situ observation of dissolved gases and volatile organic compounds in aquatic environments. Its design maintains excellent low mass range sensitivity and stability during long-term operations, enabling characterization of low-frequency variability in many trace dissolved gases. Results are presented from laboratory trials and a 300-h in situ trial in a shallow marine embayment in Massachusetts, U.S.A. This time series consists of over 15000 sample measurements and represents the longest continuous record made by an in situ mass spectrometer in an aquatic environment. These measurements possess sufficient sampling density and duration to apply frequency analysis techniques for study of temporal variability in dissolved gases. Results reveal correlations with specific environmental periodicities. Numerical methods are presented for converting mass spectrometer ion peak ratios to absolute-scale dissolved gas concentrations across wide temperature regimes irrespective of ambient pressure, during vertical water column profiles in a hypoxic deep marine basin off the coast of California, U.S.A. Dissolved oxygen concentration values obtained with the TETHYS instrument indicate close correlation with polarographic oxygen sensor data across the entire depth range. These methods and technology enable observation of aquatic environmental chemical distributions and dynamics at appropriate scales of resolution.

How the Toughest Inorganic Fullerene Cages Absorb Shockwave Pressures in a Protective Nanocomposite: Experimental Evidence from Two In Situ Investigations.

PubMed

Xu, Fang; Kobayashi, Takamichi; Yang, Zhuxian; Sekine, Toshimori; Chang, Hong; Wang, Nannan; Xia, Yongde; Zhu, Yanqiu

2017-08-22

Nanocomposites fabricated using the toughest caged inorganic fullerene WS 2 (IF-WS 2 ) nanoparticles could offer ultimate protection via absorbing shockwaves; however, if the IF-WS 2 nanomaterials really work, how they behave and what they experience within the nanocomposites at the right moment of impact have never been investigated effectively, due to the limitations of existing investigation techniques that are unable to elucidate the true characteristics of high-speed impacts in composites. We first fabricated Al matrix model nanocomposites and then unlocked the exact roles of IF-WS 2 in it at the exact moment of impact, at a time resolution that has never been attempted before, using two in situ techniques. We find that the presence of IF-WS 2 reduced the impact velocity by over 100 m/s and in pressure by at least 2 GPa against those Al and hexagonal WS 2 platelet composites at an impact speed of 1000 m/s. The IF-WS 2 composites achieved an intriguing inelastic impact and outperformed other reference composites, all originating from the "balloon effect" by absorbing the shockwave pressures. This study not only provides fundamental understanding for the dynamic performance of composites but also benefits the development of protective nanocomposite engineering.

Hydrophobic Coatings on Cotton Obtained by in Situ Plasma Polymerization of a Fluorinated Monomer in Ethanol Solutions.

PubMed

Molina, Ricardo; Teixidó, Josep Maria; Kan, Chi-Wai; Jovančić, Petar

2017-02-15

Plasma polymerization using hydrophobic monomers in the gas phase is a well-known technology to generate hydrophobic coatings. However, synthesis of functional hydrophobic coatings using plasma technology in liquids has not yet been accomplished. This work is consequently focused on polymerization of a liquid fluorinated monomer on cotton fabric initiated by atmospheric plasma in a dielectric barrier discharge configuration. Functional hydrophobic coatings on cotton were successfully achieved using in situ atmospheric plasma-initiated polymerization of fluorinated monomer dissolved in ethanol. Gravimetric measurements reveal that the amount of polymer deposited on cotton substrates can be modulated with the concentration of monomer in ethanol solution, and cross-linking reactions occur during plasma polymerization of a fluorinated monomer even without the presence of a cross-linking agent. FTIR and XPS analysis were used to study the chemical composition of hydrophobic coatings and to get insights into the physicochemical processes involved in plasma treatment. SEM analysis reveals that at high monomer concentration, coatings possess a three-dimensional pattern with a characteristic interconnected porous network structure. EDX analysis reveals that plasma polymerization of fluorinated monomers takes place preferentially at the surface of cotton fabric and negligible polymerization takes place inside the cotton fabric. Wetting time measurements confirm the hydrophobicity of cotton coatings obtained although equilibrium moisture content was slightly decreased. Additionally, the abrasion behavior and resistance to washing of plasma-coated cotton has been evaluated.

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

Multi-parameter brain tissue microsensor and interface systems: calibration, reliability and user experiences of pressure and temperature sensors in the setting of neurointensive care.

PubMed

Childs, Charmaine; Wang, Li; Neoh, Boon Kwee; Goh, Hok Liok; Zu, Mya Myint; Aung, Phyo Wai; Yeo, Tseng Tsai

2014-10-01

The objective was to investigate sensor measurement uncertainty for intracerebral probes inserted during neurosurgery and remaining in situ during neurocritical care. This describes a prospective observational study of two sensor types and including performance of the complete sensor-bedside monitoring and readout system. Sensors from 16 patients with severe traumatic brain injury (TBI) were obtained at the time of removal from the brain. When tested, 40% of sensors achieved the manufacturer temperature specification of 0.1 °C. Pressure sensors calibration differed from the manufacturers at all test pressures in 8/20 sensors. The largest pressure measurement error was in the intraparenchymal triple sensor. Measurement uncertainty is not influenced by duration in situ. User experiences reveal problems with sensor 'handling', alarms and firmware. Rigorous investigation of the performance of intracerebral sensors in the laboratory and at the bedside has established measurement uncertainty in the 'real world' setting of neurocritical care.

Atom Probe Analysis of Ex Situ Gas-Charged Stable Hydrides.

PubMed

Haley, Daniel; Bagot, Paul A J; Moody, Michael P

2017-04-01

In this work, we report on the atom probe tomography analysis of two metallic hydrides formed by pressurized charging using an ex situ hydrogen charging cell, in the pressure range of 200-500 kPa (2-5 bar). Specifically we report on the deuterium charging of Pd/Rh and V systems. Using this ex situ system, we demonstrate the successful loading and subsequent atom probe analysis of deuterium within a Pd/Rh alloy, and demonstrate that deuterium is likely present within the oxide-metal interface of a native oxide formed on vanadium. Through these experiments, we demonstrate the feasibility of ex situ hydrogen analysis for hydrides via atom probe tomography, and thus a practical route to three-dimensional imaging of hydrogen in hydrides at the atomic scale.

In situ experimental study of subduction zone fluids using diamond anvil cells

NASA Astrophysics Data System (ADS)

Bureau, H.; Foy, E.; Somogyi, A.; Munsch, P.; Simon, G.; Kubsky, S.

2008-12-01

Experiments carried out in diamond anvil cells combined with in situ synchrotron light source measurements represent the only one issue to observe and study fluid equilibria in real time, at the pressure and temperature conditions of the subduction zones. We will present new results recently obtained at the DIFFABS beam line (SOLEIL Synchrotron) aiming at studying equilibria between silica-rich hydrous melts and aqueous fluids in the presence of U, Th, Pb, Ba and Br. We used synchrotron X-Ray fluorescence analysis performed in situ in Bassett-modified hydrothermal diamond anvil cells in order to monitor the chemical transfers of the studied elements between the phases in equilibrium at different pressures (up to 1.6 GPa) and temperatures (up to 900°C). We have calculated the partition coefficients for each studied element (i): Difluid/melt = Cifluid/Cimelt. Results show that U and Th exhibit more affinities for the silica-rich hydrous fluids in the presence or absence of Br, considered here such as an analogue for Cl, (i.e. 0.4 < DUfluid/melt < 0.7 depending on P,T conditions). Br partitioning shows that whereas this halogen element has very strong affinity to the aqueous fluid during magma degassing (DBrfluid/melt >> 10 after decompression) this coefficient decreases with pressure suggesting that Br would not be immediately washed out from the subducted plate during dehydration but may be recycled deeper in the mantle. These new data combined with previous ones obtained for Pb, Ba (Bureau et al., 2007, HPR vol 27, p. 235) and Rb, Sr, Zr (Bureau et al., 2004, Eos Trans. AGU, 85(47), V11C-05), allow us to propose a general outline of the fluid phase transfers through the subduction factory: (1) at shallow level: their nature and composition, the impact of the presence of halogens and the fertilizing role of such fluids in the mantle wedge, where the generation of arc magmas takes place (2) deeper in the mantle: where hydrous silica-rich supercritical fluids may

Laser techniques in high-pressure geophysics

NASA Technical Reports Server (NTRS)

Hemley, R. J.; Bell, P. M.; Mao, H. K.

1987-01-01

Laser techniques in conjunction with the diamond-anvil cell can be used to study high-pressure properties of materials important to a wide range of problems in earth and planetary science. Spontaneous Raman scattering of crystalline and amorphous solids at high pressure demonstrates that dramatic changes in structure and bonding occur on compression. High-pressure Brillouin scattering is sensitive to the pressure variations of single-crystal elastic moduli and acoustic velocities. Laser heating techniques with the diamond-anvil cell can be used to study phase transitions, including melting, under deep-earth conditions. Finally, laser-induced ruby fluorescence has been essential for the development of techniques for generating the maximum pressures now possible with the diamond-anvil cell, and currently provides a calibrated in situ measure of pressure well above 100 gigapascals.

Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions.

PubMed

Richard, M-I; Fernández, S; Hofmann, J P; Gao, L; Chahine, G A; Leake, S J; Djazouli, H; De Bortoli, Y; Petit, L; Boesecke, P; Labat, S; Hensen, E J M; Thomas, O; Schülli, T

2017-09-01

A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10 -2 -10 3 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

Acoustic and mechanical response of reservoir rocks under variable saturation and effective pressure.

PubMed

Ravazzoli, C L; Santos, J E; Carcione, J M

2003-04-01

We investigate the acoustic and mechanical properties of a reservoir sandstone saturated by two immiscible hydrocarbon fluids, under different saturations and pressure conditions. The modeling of static and dynamic deformation processes in porous rocks saturated by immiscible fluids depends on many parameters such as, for instance, porosity, permeability, pore fluid, fluid saturation, fluid pressures, capillary pressure, and effective stress. We use a formulation based on an extension of Biot's theory, which allows us to compute the coefficients of the stress-strain relations and the equations of motion in terms of the properties of the single phases at the in situ conditions. The dry-rock moduli are obtained from laboratory measurements for variable confining pressures. We obtain the bulk compressibilities, the effective pressure, and the ultrasonic phase velocities and quality factors for different saturations and pore-fluid pressures ranging from normal to abnormally high values. The objective is to relate the seismic and ultrasonic velocity and attenuation to the microstructural properties and pressure conditions of the reservoir. The problem has an application in the field of seismic exploration for predicting pore-fluid pressures and saturation regimes.

Molecular Tagging Velocimetry Development for In-situ Measurement in High-Temperature Test Facility

NASA Technical Reports Server (NTRS)

Andre, Matthieu A.; Bardet, Philippe M.; Burns, Ross A.; Danehy, Paul M.

2015-01-01

The High Temperature Test Facility, HTTF, at Oregon State University (OSU) is an integral-effect test facility designed to model the behavior of a Very High Temperature Gas Reactor (VHTR) during a Depressurized Conduction Cooldown (DCC) event. It also has the ability to conduct limited investigations into the progression of a Pressurized Conduction Cooldown (PCC) event in addition to phenomena occurring during normal operations. Both of these phenomena will be studied with in-situ velocity field measurements. Experimental measurements of velocity are critical to provide proper boundary conditions to validate CFD codes, as well as developing correlations for system level codes, such as RELAP5 (http://www4vip.inl.gov/relap5/). Such data will be the first acquired in the HTTF and will introduce a diagnostic with numerous other applications to the field of nuclear thermal hydraulics. A laser-based optical diagnostic under development at The George Washington University (GWU) is presented; the technique is demonstrated with velocity data obtained in ambient temperature air, and adaptation to high-pressure, high-temperature flow is discussed.

Comparison of Niskin vs. in situ approaches for analysis of gene expression in deep Mediterranean Sea water samples

NASA Astrophysics Data System (ADS)

Edgcomb, V. P.; Taylor, C.; Pachiadaki, M. G.; Honjo, S.; Engstrom, I.; Yakimov, M.

2016-07-01

Obtaining an accurate picture of microbial processes occurring in situ is essential for our understanding of marine biogeochemical cycles of global importance. Water samples are typically collected at depth and returned to the sea surface for processing and downstream experiments. Metatranscriptome analysis is one powerful approach for investigating metabolic activities of microorganisms in their habitat and which can be informative for determining responses of microbiota to disturbances such as the Deepwater Horizon oil spill. For studies of microbial processes occurring in the deep sea, however, sample handling, pressure, and other changes during sample recovery can subject microorganisms to physiological changes that alter the expression profile of labile messenger RNA. Here we report a comparison of gene expression profiles for whole microbial communities in a bathypelagic water column sample collected in the Eastern Mediterranean Sea using Niskin bottle sample collection and a new water column sampler for studies of marine microbial ecology, the Microbial Sampler - In Situ Incubation Device (MS-SID). For some taxa, gene expression profiles from samples collected and preserved in situ were significantly different from potentially more stressful Niskin sampling and preservation on deck. Some categories of transcribed genes also appear to be affected by sample handling more than others. This suggests that for future studies of marine microbial ecology, particularly targeting deep sea samples, an in situ sample collection and preservation approach should be considered.

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.

Quantification of in situ pore pressure and stress in regions of low frequency earthquakes and anomalously low seismic velocity at the Nankai Trough

NASA Astrophysics Data System (ADS)

Kitajima, H.; Saffer, D. M.

2012-12-01

Recent seismic reflection and ocean bottom seismometer (OBS) studies reveal broad regions of low seismic velocity along the megathrust plate boundary of the Nankai subduction zone offshore SW Japan. These low velocity zones (LVZ's) extend to ~55 km from the trench, corresponding to depths of >~10 km below sea floor. Elevated pore pressure has been invoked as one potential cause of both the LVZ's and very low frequency earthquakes (VLFE) in the outer forearc. Here, we estimate the in-situ pore fluid pressure and stress state within these LVZ's by combining P-wave velocities (Vp) obtained from seismic reflection and OBS data with well-constrained empirical relations between (1) P-wave velocity and porosity; and (2) porosity and effective mean and differential stresses, defined by triaxial deformation tests on drill core samples of the incoming oceanic sediment. We used cores of Lower Shikoku Basin (LSB) hemipelagic mudstone (322-C0011B-19R-5, initial porosity of 43%), and Middle Shikoku Basin (MSB) tuffaceous sandstone (333-C0011D-51X-2, initial porosity of 46%) that have been recovered from IODP Nankai Trough Seismogenic Zone Experiment (NanTroSEIZE) Site C0011 (~20 km seaward from the deformation front). Samples were loaded under a range of different stress paths including isotropic loading, triaxial compression, and triaxial extension. During the tests, all pressures, axial displacement, and pore volume change were continuously monitored; and ultrasonic velocity and permeability were measured at regular intervals. The relationship between Vp and porosity for LSB mudstone is independent of stress path, and is well fit by an empirical function derived by Hoffman and Tobin [2004] for LSB sediments sampled by drilling along Muroto transect, located ~150 km southwest of the NanTroSEIZE study area. The MSB sandstone exhibits slightly higher P-wave velocity than LSB mudstone at a given porosity. Based on our experimental results, and assuming that the sediments in the

In-situ visual observation for the formation and dissociation of methane hydrates in porous media by magnetic resonance imaging.

PubMed

Zhao, Jiafei; Lv, Qin; Li, Yanghui; Yang, Mingjun; Liu, Weiguo; Yao, Lei; Wang, Shenglong; Zhang, Yi; Song, Yongchen

2015-05-01

In this work, magnetic resonance imaging (MRI) was employed to observe the in-situ formation and dissociation of methane hydrates in porous media. Methane hydrate was formed in a high-pressure cell with controlled temperature, and then the hydrate was dissociated by thermal injection. The process was photographed by the MRI, and the pressure was recorded. The images confirmed that the direct visual observation was achieved; these were then employed to provide detailed information of the nucleation, growth, and decomposition of the hydrate. Moreover, the saturation of methane hydrate during the dissociation was obtained from the MRI intensity data. Our results showed that the hydrate saturation initially decreased rapidly, and then slowed down; this finding is in line with predictions based only on pressure. The study clearly showed that MRI is a useful technique to investigate the process of methane hydrate formation and dissociation in porous media. Copyright © 2015 Elsevier Inc. All rights reserved.

Mass-induced sea level variations in the Red Sea from GRACE, steric-corrected altimetry, in situ bottom pressure records, and hydrographic observations

NASA Astrophysics Data System (ADS)

Feng, W.; Lemoine, J.-M.; Zhong, M.; Hsu, H. T.

2014-08-01

An annual amplitude of ∼18 cm mass-induced sea level variations (SLV) in the Red Sea is detected from the Gravity Recovery and Climate Experiment (GRACE) satellites and steric-corrected altimetry from 2003 to 2011. The annual mass variations in the region dominate the mean SLV, and generally reach maximum in late January/early February. The annual steric component of the mean SLV is relatively small (<3 cm) and out of phase of the mass-induced SLV. In situ bottom pressure records at the eastern coast of the Red Sea validate the high mass variability observed by steric-corrected altimetry and GRACE. In addition, the horizontal water mass flux of the Red Sea estimated from GRACE and steric-corrected altimetry is validated by hydrographic observations.

Ultrasonication aided in-situ transesterification of microbial lipids to biodiesel.

PubMed

Zhang, Xiaolei; Yan, Song; Tyagi, Rajeshwar Dayal; Surampalli, Rao Y; Valéro, Jose R

2014-10-01

In-situ transesterification of microbial lipid to biodiesel has been paid substantial attention due to the fact that the lipid extraction and transesterification can be conducted in one-stage process. To improve the feasibility of in-situ transesterification, ultrasonication was employed to reduce methanol requirement and reaction time. The results showed that the use of ultrasonication could achieve high conversion of lipid to FAMEs (92.1% w lipid conversion/w total lipids) with methanol to lipid molar ratio 60:1 and NaOH addition 1% w/w lipid in 20 min, while methanol to lipid molar ratio 360:1, NaOH addition 1% w/w lipid, and reaction time 12h was required to obtain similar yield in in-situ transesterification without ultrasonication. The compositions of FAMEs obtained in case of ultrasonication aided in-situ transesterification were similar as that of two-stage extraction followed by transesterification processes. Copyright © 2014. Published by Elsevier Ltd.

Steady- and unsteady-pressure measurements on a supercritical-wing model with oscillating control surfaces at subsonic and transonic speeds

NASA Technical Reports Server (NTRS)

Sandford, M. C.; Ricketts, R. H.

1983-01-01

A high aspect ratio supercritical wing with oscillating control surfaces is described. The semispan wing model was instrumented with 252 static pressure orifices and 164 in situ dynamic pressure gages for studying the effects of control surface position and sinusoidal motion on steady and unsteady pressures. Results from the present test (the third in a series of tests on this model) were obtained in the Langley Transonic Dynamics Tunnel at Mach numbers of 0.60, 0.78, and 0.86 and are presented in tabular form.

Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

2017-06-01

A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

The Detached Auroras Induced by the Solar Wind Pressure Enhancement in Both Hemispheres From Imaging and In Situ Particle Observations

NASA Astrophysics Data System (ADS)

Zhou, Su; Luan, Xiaoli; Søraas, Finn; Østgaard, Nikolai; Raita, Tero

2018-04-01

This paper presents simultaneous detached proton auroras that appeared in both hemispheres at 11:06 UT, 08 March 2012, just 2 min after a sudden solar wind pressure enhancement ( 11:04 UT) hit the Earth. They were observed under northward interplanetary magnetic field Bz condition and during the recovery phase of a moderate geomagnetic storm. In the Northern Hemisphere, Defense Meteorological Satellite Program/Special Sensor Ultraviolet Spectrographic Imager observed that the detached arc occurred within 60°-65° magnetic latitude and covered a few magnetic local time (MLT) hours ranging from 0530 to 0830 MLT with a possible extension toward noon. At the same time (11:06 UT), Polar Orbiting Environment Satellites 19 detected a detached proton aurora around 1300 MLT in the Southern Hemisphere, centering 62° magnetic latitude, which was at the same latitudes as the northern detached arc. This southern aurora was most probably a part of a dayside detached arc that was conjugate to the northern one. In situ particle observations indicated that the detached auroras were dominated by protons/ions with energies ranging from around 20 keV to several hundreds of keV, without obvious electron precipitations. These detached arcs persisted for less than 6 min, consistent with the impact from pressure enhancement and the observed electromagnetic ion cyclotron (EMIC) waves. It is suggested that the increasing solar wind pressure pushed the hot ions in the ring current closer to Earth where the steep gradient of cold plasma favored EMIC wave growth. By losing energy to EMIC waves the energetic protons (>20 keV) were scattered into the loss cone and produced the observed detached proton auroras.

Deformation of olivine under mantle conditions: An in situ high-pressure, high-temperature study using monochromatic synchrotron radiation

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

Hilairet, Nadège; Wang, Yanbin; Sanehira, Takeshi

2012-03-15

Polycrystalline samples of San Carlos olivine were deformed at high-pressure (2.8-7.8 GPa), high-temperature (1153 to 1670 K), and strain rates between 7.10{sup -6} and 3.10{sup -5} s{sup -1}, using the D-DIA apparatus. Stress and strain were measured in situ using monochromatic X-rays diffraction and imaging, respectively. Based on the evolution of lattice strains with total bulk strain and texture development, we identified three deformation regimes, one at confining pressures below 3-4 GPa, one above 4 GPa, both below 1600 K, and one involving growth of diffracting domains associated with mechanical softening above {approx}1600 K. The softening is interpreted as enhancedmore » grain boundary migration and recovery. Below 1600 K, elasto-plastic self-consistent analysis suggests that below 3-4 GPa, deformation in olivine occurs with large contribution from the so-called 'a-slip' system [100](010). Above {approx}4 GPa, the contribution of the a-slip decreases relative to that of the 'c-slip' [001](010). This conclusion is further supported by texture refinements. Thus for polycrystalline olivine, the evolution in slip systems found by previous studies may be progressive, starting from as low as 3-4 GPa and up to 8 GPa. During such a gradual change, activation volumes measured on polycrystalline olivine cannot be linked to a particular slip system straightforwardly. The quest for 'the' activation volume of olivine at high pressure should cease at the expense of detailed work on the flow mechanisms implied. Such evolution in slip systems should also affect the interpretation of seismic anisotropy data in terms of upper mantle flow between 120 and 300 km depth.« less

Pressure-induced phase transition in GaN nanocrystals

NASA Astrophysics Data System (ADS)

Cui, Q.; Pan, Y.; Zhang, W.; Wang, X.; Zhang, J.; Cui, T.; Xie, Y.; Liu, J.; Zou, G.

2002-11-01

High-pressure in situ energy-dispersive x-ray diffraction experiments on GaN nanocrystals with 50 nm diameter have been carried out using a synchrotron x-ray source and a diamond-anvil cell up to about 79 GPa at room temperature. A pressure-induced first-order structural phase transition from the wurtzite-type structure to the rock-salt-type structure starts at about 48.8 GPa. The rock-salt-type phase persists to the highest pressure in our experimental range.

Intrinsic stress in ZrN thin films: Evaluation of grain boundary contribution from in situ wafer curvature and ex situ x-ray diffraction techniques

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

Koutsokeras, L. E.; Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110; Abadias, G.

2012-05-01

Low-mobility materials, like transition metal nitrides, usually undergo large residual stress when sputter-deposited as thin films. While the origin of stress development has been an active area of research for high-mobility materials, atomistic processes are less understood for low-mobility systems. In the present work, the contribution of grain boundary to intrinsic stress in reactively magnetron-sputtered ZrN films is evaluated by combining in situ wafer curvature measurements, providing information on the overall biaxial stress, and ex situ x-ray diffraction, giving information on elastic strain (and related stress) inside crystallites. The thermal stress contribution was also determined from the in situ stressmore » evolution during cooling down, after deposition was stopped. The stress data are correlated with variations in film microstructure and growth energetics, in the 0.13-0.42 Pa working pressure range investigated, and discussed based on existing stress models. At low pressure (high energetic bombardment conditions), a large compressive stress is observed due to atomic peening, which induces defects inside crystallites but also promotes incorporation of excess atoms in the grain boundary. Above 0.3-0.4 Pa, the adatom surface mobility is reduced, leading to the build-up of tensile stress resulting from attractive forces between under-dense neighbouring column boundary and possible void formation, while crystallites can still remain under compressive stress.« less

In situ detection of tropospheric OH, HO2, NO2, and NO by laser-induced fluorescence in detection chambers at reduced pressures

NASA Technical Reports Server (NTRS)

Brune, William H.

1993-01-01

This report is a brief summary of the status of work on the grant entitled 'In situ detection of tropospheric OH, HO2, NO2, and NO by laser induced fluorescence in detection chambers at low pressures.' The basic instrument characteristics have been established, and have been reported in a manuscript, included as an appendix to this report, that has been accepted by the Journal of Geophysical Research. Currently, two efforts are under way. First, instrument tests and calibrations are continuing. These efforts include field measurements and an informal inter comparison in Colorado last August and September. Second, new technologies in lasers and detectors are being implemented to make the instrument smaller, lighter, and more energy efficient. Such instrument modifications are essential for measurements from aircraft, high scaffolding in forests, and ships.

In-Situ Ultra Low Frequency Poroelastic Response of a Natural Macro-Fracture

NASA Astrophysics Data System (ADS)

Guglielmi, Y.; Cappa, F.; Rutqvist, J.; Tsang, C.; Gaffet, S.

2008-12-01

The seismic visibility of macro-fractures filled with fluids is a central problem in the exploration of thermo- hydro-mechanical and chemical processes that occur in Earth' s subsurface. Most studies have been concerned (1) with cracks of a small size relative to the seismic wavelength (2) with "core-sized" samples of single macro-fractures. In comparison, in-situ studies of macro-fractures are very rare and no real estimate is made of the relevance of this convenient "core-sized" data to in-situ reservoirs in general. In this study, we present a new experimental approach to in-situ characterize mechanical and hydraulic properties of fractures using the innovative HPPP protocol. This protocol allows simultaneous high-frequency (120.2 Hz) sampling of normal displacement and fluid pressure in a borehole intersecting the fracture. We show preliminary results conducted in a single fracture vertically embedded in a carbonate reservoir that contains 3 sets of macro-fractures with an average 2m spacing. Two HPPP probes were set, spaced one meter vertically in the fracture. Two types of ULF seismic sources are applied: a fluid pressure pulse injected in the fracture and a hammer hit at a point located 5m far from the fracture plane. There is a highly non-linear variation of fracture normal displacement-versus- fluid pressure as a function of frequency, the higher the frequency, the lower the displacement spectral amplitude is. The pressure pulse and the hammer hit allow exploring the fracture poroelastic response in the [0 - 3Hz] frequency range. The fracture plays the role of a "low-pass" filter for fluid pressure waves; only a quasi-static pressure signal being registered at the receiver. The displacement wave propagation is more complex resulting in uncoupled quasi-static-pressure-2Hz-deformation signals at the receiver. For low magnitude seismic sources (low amplitude pulse and seismic wave), the fracture natural resonance is amplified resulting in separate signals

Wind Tunnel Application of a Pressure-Sensitive Paint Technique to a Faceted Missile Model at Subsonic and Transonic Speeds

NASA Technical Reports Server (NTRS)

Erickson, Gary E.

2004-01-01

A pressure-sensitive paint (PSP) technique was applied in a wind tunnel experiment in the NASA Langley Research Center 8-Foot Transonic Pressure Tunnel to quantify the vortex-induced surface static pressures on a slender, faceted missile model at subsonic and transonic speeds. Global PSP calibrations were obtained using an in-situ method featuring the simultaneous electronically-scanned pressures (ESP) measurements. Both techniques revealed the significant influence leading-edge vortices on the surface pressure distributions. The mean error in the PSP measurements relative to the ESP data was approximately 0.6 percent at M(sub infinity)=0.70 and 2.6 percent at M(sub infinity)=0.90 and 1.20. The vortex surface pressure signatures obtained from the PSP and ESP techniques were correlated with the off-surface vortex cross-flow structures obtained using a laser vapor screen (LVS) flow visualization technique. The on-surface and off-surface techniques were complementary, since each provided details of the vortex-dominated flow that were not clear or apparent in the other.

Thermochromic microcapsules with highly transparent shells obtained through in-situ polymerization of urea formaldehyde around thermochromic cores for smart wood coatings.

PubMed

Zhu, Xiaodong; Liu, Yu; Li, Zhao; Wang, Weicong

2018-03-05

In this paper, thermochromic microcapsules were synthesized in situ polymerization with urea formaldehyde as shell material and thermochromic compounds as core material. The effects of emulsifying agent and conditions on surface morphology and particle size of microcapsules were studied. It was found that the size and surface morphology of microcapsules were strongly depending on stirring rate and the ratio of core to shell. The stable and small size spherical microcapsules with excellent transparency can be obtained at an emulsifying agent to core to shell ratio as 1:5:7.5 under mechanical stirring at 12 krpm for 15 min. Finally, the thermochromic property was discussed by loading microcapsules in wood and wood coatings. Results indicate that microcapsules can realize the thermochromic property while incorporated with wood and coatings, and could have high potential in smart material fabrication.

Method for obtaining large levitation pressure in superconducting magnetic bearings

DOEpatents

Hull, John R.

1997-01-01

A method and apparatus for compressing magnetic flux to achieve high levitation pressures. Magnetic flux produced by a magnetic flux source travels through a gap between two high temperature superconducting material structures. The gap has a varying cross-sectional area to compress the magnetic flux, providing an increased magnetic field and correspondingly increased levitation force in the gap.

Method for obtaining large levitation pressure in superconducting magnetic bearings

DOEpatents

Hull, John R.

1996-01-01

A method and apparatus for compressing magnetic flux to achieve high levitation pressures. Magnetic flux produced by a magnetic flux source travels through a gap between two high temperature superconducting material structures. The gap has a varying cross-sectional area to compress the magnetic flux, providing an increased magnetic field and correspondingly increased levitation force in the gap.

In-situ XRD vs ex-situ vacuum annealing of tantalum oxynitride thin films: Assessments on the structural evolution

NASA Astrophysics Data System (ADS)

Cunha, L.; Apreutesei, M.; Moura, C.; Alves, E.; Barradas, N. P.; Cristea, D.

2018-04-01

The purpose of this work is to discuss the main structural characteristics of a group of tantalum oxynitride (TaNxOy) thin films, with different compositions, prepared by magnetron sputtering, and to interpret and compare the structural changes, by X-ray diffraction (XRD), when the samples are vacuum annealed under two different conditions: i) annealing, followed by ex-situ XRD: one sample of each deposition run was annealed at a different temperature, until a maximum of 800 °C, and the XRD patterns were obtained, at room temperature, after each annealing process; ii) annealing with in-situ XRD: the diffraction patterns are obtained, at certain temperatures, during the annealing process, using always the same sample. In-situ XRD annealing could be an interesting process to perform annealing, and analysing the evolution of the structure with the temperature, when compared to the classical process. A higher structural stability was observed in some of the samples, particularly on those with highest oxygen content, but also on the sample with non-metal (O + N) to metal (Ta) ratio around 0.5.

Enhanced Stability of Pt-Cu Single-Atom Alloy Catalysts: In Situ Characterization of the Pt/Cu(111) Surface in an Ambient Pressure of CO

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

Simonovis, Juan Pablo; Hunt, Adrian; Palomino, Robert M.

The interaction between a catalyst and reactants often induce changes in the surface structure and composition of the catalyst, which, in turn, affect its reactivity. Therefore, it is important to study such changes using in situ techniques under well-controlled conditions. We have used ambient pressure X-ray photoelectron spectroscopy (AP-XPS) to study the surface stability of a Pt/Cu(111) single atom alloy (SAA) in an ambient pressure of CO. By directly probing the Pt atoms, we found that CO causes a slight surface segregation of Pt atoms at room temperature. In addition, while the Pt/Cu(111) surface demonstrates poor thermal stability in UHV,more » where surface Pt starts to diffuse to the subsurface layer above 400 K, the presence of adsorbed CO enhances the thermal stability of surface Pt atoms. Furthermore, we also found that temperatures above 450 K cause a restructuring of the subsurface layer, which consequently strengthens the CO binding to the surface Pt sites, likely due to the presence of neighboring subsurface Pt atoms.« less

Enhanced Stability of Pt-Cu Single-Atom Alloy Catalysts: In Situ Characterization of the Pt/Cu(111) Surface in an Ambient Pressure of CO

DOE PAGES

Simonovis, Juan Pablo; Hunt, Adrian; Palomino, Robert M.; ...

2018-02-05

The interaction between a catalyst and reactants often induce changes in the surface structure and composition of the catalyst, which, in turn, affect its reactivity. Therefore, it is important to study such changes using in situ techniques under well-controlled conditions. We have used ambient pressure X-ray photoelectron spectroscopy (AP-XPS) to study the surface stability of a Pt/Cu(111) single atom alloy (SAA) in an ambient pressure of CO. By directly probing the Pt atoms, we found that CO causes a slight surface segregation of Pt atoms at room temperature. In addition, while the Pt/Cu(111) surface demonstrates poor thermal stability in UHV,more » where surface Pt starts to diffuse to the subsurface layer above 400 K, the presence of adsorbed CO enhances the thermal stability of surface Pt atoms. Furthermore, we also found that temperatures above 450 K cause a restructuring of the subsurface layer, which consequently strengthens the CO binding to the surface Pt sites, likely due to the presence of neighboring subsurface Pt atoms.« less

In situ spray deposition of cell-loaded, thermally and chemically gelling hydrogel coatings for tissue regeneration.

PubMed

Pehlivaner Kara, Meryem O; Ekenseair, Adam K

2016-10-01

In this study, the efficacy of creating cellular hydrogel coatings on warm tissue surfaces through the minimally invasive, sprayable delivery of thermoresponsive liquid solutions was investigated. Poly(N-isopropylacrylamide)-based (pNiPAAm) thermogelling macromers with or without addition of crosslinking polyamidoamine (PAMAM) macromers were synthesized and used to produce in situ forming thermally and chemically gelling hydrogel systems. The effect of solution and process parameters on hydrogel physical properties and morphology was evaluated and compared to poly(ethylene glycol) and injection controls. Smooth, fast, and conformal hydrogel coatings were obtained when pNiPAAm thermogelling macromers were sprayed with high PAMAM concentration at low pressure. Cellular hydrogel coatings were further fabricated by different spraying techniques: single-stream, layer-by-layer, and dual stream methods. The impact of spray technique, solution formulation, pressure, and spray solution viscosity on the viability of fibroblast and osteoblast cells encapsulated in hydrogels was elucidated. In particular, the early formation of chemically crosslinked micronetworks during bulk liquid flow was shown to significantly affect cell viability under turbulent conditions compared to injectable controls. The results demonstrated that sprayable, in situ forming hydrogels capable of delivering cell populations in a homogeneous therapeutic coating on diseased tissue surfaces offer promise as novel therapies for applications in regenerative medicine. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2383-2393, 2016. © 2016 Wiley Periodicals, Inc.

Variabilities detected by acoustic emission from filament-wound Aramid fiber/epoxy composite pressure vessels

NASA Technical Reports Server (NTRS)

Hamstad, M. A.

1978-01-01

Two hundred and fifty Aramid fiber/epoxy pressure vessels were filament-wound over spherical aluminum mandrels under controlled conditions typical for advanced filament-winding. A random set of 30 vessels was proof-tested to 74% of the expected burst pressure; acoustic emission data were obtained during the proof test. A specially designed fixture was used to permit in situ calibration of the acoustic emission system for each vessel by the fracture of a 4-mm length of pencil lead (0.3 mm in diameter) which was in contact with the vessel. Acoustic emission signatures obtained during testing showed larger than expected variabilities in the mechanical damage done during the proof tests. To date, identification of the cause of these variabilities has not been determined.

Method for obtaining large levitation pressure in superconducting magnetic bearings

DOEpatents

Hull, J.R.

1997-08-05

A method and apparatus are disclosed for compressing magnetic flux to achieve high levitation pressures. Magnetic flux produced by a magnetic flux source travels through a gap between two high temperature superconducting material structures. The gap has a varying cross-sectional area to compress the magnetic flux, providing an increased magnetic field and correspondingly increased levitation force in the gap. 4 figs.

Method for obtaining large levitation pressure in superconducting magnetic bearings

DOEpatents

Hull, J.R.

1996-10-08

A method and apparatus are disclosed for compressing magnetic flux to achieve high levitation pressures. Magnetic flux produced by a magnetic flux source travels through a gap between two high temperature superconducting material structures. The gap has a varying cross-sectional area to compress the magnetic flux, providing an increased magnetic field and correspondingly increased levitation force in the gap. 4 figs.

In situ detection of porosity initiation during aluminum thin film anodizing

NASA Astrophysics Data System (ADS)

Van Overmeere, Quentin; Nysten, Bernard; Proost, Joris

2009-02-01

High-resolution curvature measurements have been performed in situ during aluminum thin film anodizing in sulfuric acid. A well-defined transition in the rate of internal stress-induced curvature change is shown to allow for the accurate, real-time detection of porosity initiation. The validity of this in situ diagnostic tool was confirmed by a quantitative analysis of the spectral density distributions of the anodized surfaces. These were obtained by analyzing ex situ atomic force microscopy images of surfaces anodized for different times, and allowed to correlate the in situ detected transition in the rate of curvature change with the appearance of porosity.

Development of a double-stage DDIA apparatus and its application to in-situ melting experiments at high pressures

NASA Astrophysics Data System (ADS)

Jing, Z.; Wang, Y.; Tange, Y.; Hilairet, N.; Yu, T.; Sakamaki, T.

2010-12-01

Melting experiments at high pressures are critical to our studies on the chemical evolution and dynamics of Earth and other terrestrial planets. A large volume press can generate a homogeneous and stable high-temperature environment, which is the key to melting experiments. However, previous in-situ melting experiments using a large volume press were often restricted to relatively low pressures. In order to expand the P-T conditions, a double-stage 6-8 configuration (6 first-stage anvils and 8 second stage-anvils) has been developed in a DDIA apparatus (DDIA-30), recently installed at the GSECARS Beamline 13-ID-D at the Advanced Photon Source. 27 mm DIA-type first-stage anvils and 14 mm second-stage anvils with the truncation edge length (TEL) of 1.5 mm are employed. A cell assembly that is suitable for synchrotron X-ray studies developed by Tange et al. (2008) has been adopted for melting experiments. High pressure and temperature conditions are generated up to 27 GPa and 2473 K by using tungsten carbide anvils, and up to 35 GPa and 1773 K by using sintered diamond anvils. Both LaCrO3 and TiB2 heater materials have been successfully applied for high-temperature generation. Although TiB2 shows a decrease of resistance at temperatures higher than 2000 K at 20 GPa, we are able to achieve 2473 K with temperature fluctuations in the range of ±30 K. Using tungsten carbide anvils and TiB2 heaters, we have determined the melting curve of gold up to 20 GPa. We constrain the melting temperature based on the disappearance of the gold peaks in energy dispersive X-ray diffraction patterns and the change of sample shape in the radiographic images. The combination of these two observations can reduce the uncertainties in melting temperatures to within 100 K. The measured melting temperatures of gold at 8, 13, and 20 GPa are consistent with the low-pressure results (up to 6 GPa) such as Mirwald and Kennedy (1979). Melting experiments with sintered diamond anvils are currently

Integrated in-situ probes for structural and dynamic properties of geological materials at ultrahigh pressures and temperatures

NASA Astrophysics Data System (ADS)

Mao, H.; Mao, W. L.

2005-12-01

Multiple x-ray and allied probes have been recently developed and integrated with diamond-anvil cells at synchrotron facilities. They have effectively opened up the vast field area of the Earth's interior to direct, in-situ study. For instance, x-ray emission spectroscopy identifies the high-spin-low-spin transition that governs Fe-Mg partitioning, the most important factor in element differentiation in the mantle. Inelastic x-ray near-edge spectroscopy reveals the bonding nature of light elements that control the phase transitions, structure and partitioning of these elements (e.g., carbon bonding changes as an element, and in oxides, carbonates, and silicates). X-ray diffraction combined with laser-heated diamond anvil cell determines crystal structures and P-V-T equations of state. Shear moduli, single-crystal elasticity, and phonon dynamics can be measured to the core pressures with newly-enabled, complementary techniques, including radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, non-resonant inelastic x-ray scattering, high-temperature Raman spectroscopy, and Brillouin scattering spectroscopy. The nonhydrostatic stress in solid samples which was previously regarded as a nuisance that degraded the experiments, can now be used for extracting important rheological information, including deformation mechanisms, preferred orientation, slip systems, plasticity, failure, and shear strength of major mantle and core minerals at high pressures. With the new arsenal of experimental techniques over the extended P-T-x regimes at we can now address questions that were not conceivable only a decade ago. Knowledge of the high P-T properties is leading to fundamental improvements in interpreting seismological observations and understanding the structure, dynamics, and evolution of the Earth's deep interior.

Subsonic and transonic pressure measurements on a high-aspect-ratio supercritical-wing model with oscillating control surfaces

NASA Technical Reports Server (NTRS)

Sandford, M. C.; Ricketts, R. H.; Watson, J. J.

1981-01-01

A high aspect ratio supercritical wing with oscillating control surfaces is described. The semispan wing model was instrumented with 252 static orifices and 164 in situ dynamic pressure gases for studying the effects of control surface position and sinusoidal motion on steady and unsteady pressures. Data from the present test (this is the second in a series of tests on this model) were obtained in the Langley Transonic Dynamics Tunnel at Mach numbers of 0.60 and 0.78 and are presented in tabular form.

Effects of hydrostatic pressure on microbial alteration of sinking fecal pellets

NASA Astrophysics Data System (ADS)

Tamburini, Christian; Goutx, Madeleine; Guigue, Catherine; Garel, Marc; Lefèvre, Dominique; Charrière, Bruno; Sempéré, Richard; Pepa, Stéphane; Peterson, Michael L.; Wakeham, Stuart; Lee, Cindy

2009-08-01

We used a new experimental device called PASS (PArticle Sinking Simulator) during MedFlux to simulate changes in in situ hydrostatic pressure that particles experience sinking from mesopelagic to bathypelagic depths. Particles, largely fecal pellets, were collected at 200 m using a settling velocity NetTrap (SV NetTrap) in Ligurian Sea in April 2006 and incubated in high-pressure bottles (HPBs) of the PASS system under both atmospheric and continuously increasing pressure conditions, simulating the pressure change experienced at a sinking rate of 200 m d -1. Chemical changes over time were evaluated by measuring particulate organic carbon (POC), carbohydrates, transparent exopolymer particles (TEP), amino acids, lipids, and chloropigments, as well as dissolved organic carbon (DOC) and dissolved carbohydrates. Microbial changes were evaluated microscopically, using diamidinophenylindole (DAPI) stain for total cell counts and catalyzed reporter deposition-fluorescence in situ hybridization (CARD-FISH) for phylogenetic distinctions. Concentrations (normalized to POC) of particulate chloropigments, carbohydrates and TEP decreased under both sets of incubation conditions, although less under the increasing pressure regime than under atmospheric conditions. By contrast, dissolved carbohydrates (normalized to DOC) were higher after incubation and significantly higher under atmospheric conditions, suggesting they were produced at the expense of the particulate fraction. POC-normalized particulate wax/steryl esters increased only under pressure, suggesting biochemical responses of prokaryotes to the increasing pressure regime. The prokaryotic community initially consisted of 43% Bacteria, 12% Crenarchaea and 11% Euryarchaea. After incubation, Bacteria dominated (˜90%) the prokaryote community in all cases, with γ- Proteobacteria comprising the greatest fraction, followed by the Cytophaga-Flavobacter cluster and α -Proteobacteria group. Using the PASS system, we obtained

Prokaryotic responses to hydrostatic pressure in the ocean--a review.

PubMed

Tamburini, Christian; Boutrif, Mehdi; Garel, Marc; Colwell, Rita R; Deming, Jody W

2013-05-01

Effects of hydrostatic pressure on pure cultures of prokaryotes have been studied extensively but impacts at the community level in the ocean are less well defined. Here we consider hydrostatic pressure effects on natural communities containing both unadapted (piezosensitive) prokaryotes originating from surface water and adapted (including piezophilic) prokaryotes from the deep sea. Results from experiments mimicking pressure changes experienced by particle-associated prokaryotes during their descent through the water column show that rates of degradation of organic matter (OM) by surface-originating microorganisms decrease with sinking. Analysis of a much larger data set shows that, under stratified conditions, deep-sea communities adapt to in situ conditions of high pressure, low temperature and low OM. Measurements made using decompressed samples and atmospheric pressure thus underestimate in situ activity. Exceptions leading to overestimates can be attributed to deep mixing events, large influxes of surface particles, or provision of excessive OM during experimentation. The sediment-water interface, where sinking particles accumulate, will be populated by a mixture of piezosensitive, piezotolerant and piezophilic prokaryotes, with piezophilic activity prevailing deeper within sediment. A schematic representation of how pressure shapes prokaryotic communities in the ocean is provided, allowing a reasonably accurate interpretation of the available activity measurements. © 2013 Society for Applied Microbiology and Blackwell Publishing Ltd.

In situ detection of tropospheric OH, HO2, NO2, and NO by laser-induced fluorescence in detection chambers at reduced pressures

NASA Technical Reports Server (NTRS)

Brune, William H.

1992-01-01

This report is a brief summary of the status of work on the grant entitled 'In situ detection of tropospheric OH, HO2, NO2, and NO by laser induced fluorescence in detection chambers at low pressures'. The first version of the instrument is essentially complete and operational for about six months, and we continue to make improvements on the instrument sensitivity and reliability. We are focusing our efforts on improving our understanding of the operating characteristics of the instrument - particularly the inlet transmission for OH and HO2, the exact character of the air flow around and within the instrument, and the efficiency of the chemical conversion of HO2 to OH. We are also in the process of converting this laboratory instrument into a field worthy instrument that we can take to remote sites for measurements.

Pressure sensor

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

Mee, David K.; Ripley, Edward B.; Nienstedt, Zachary C.

Disclosed is a passive, in-situ pressure sensor. The sensor includes a sensing element having a ferromagnetic metal and a tension inducing mechanism coupled to the ferromagnetic metal. The tension inducing mechanism is operable to change a tensile stress upon the ferromagnetic metal based on a change in pressure in the sensing element. Changes in pressure are detected based on changes in the magnetic switching characteristics of the ferromagnetic metal when subjected to an alternating magnetic field caused by the change in the tensile stress. The sensing element is embeddable in a closed system for detecting pressure changes without the needmore » for any penetrations of the system for power or data acquisition by detecting changes in the magnetic switching characteristics of the ferromagnetic metal caused by the tensile stress.« less

A sample predictive model for intraocular pressure following laser in situ keratomileusis for myopia and an "intraocular pressure constant".

PubMed

Bahadir Kilavuzoglu, Ayse Ebru; Bozkurt, Tahir Kansu; Cosar, Cemile Banu; Sener, Asım Bozkurt

2017-06-24

To describe a sample predictive model for intraocular pressure (IOP) following laser in situ keratomileusis (LASIK) for myopia and an IOP constant. The records of patients that underwent LASIK for myopia and myopic astigmatism via WaveLight Allegretto Wave Eye-Q 400 Hz excimer laser and Hansatome XP microkeratome were retrospectively reviewed. Patients with no systemic or ocular disease other than myopia or myopic astigmatism were included in the study. Preoperative and postoperative month 1 data and intraoperative data were used to build the predictive model for IOP after LASIK. The IOP constant was calculated by subtracting the predicted IOP from preoperative IOP. The paired samples t test, Pearson's correlation analysis, curve estimation analysis, and linear regression analysis were used to evaluate the study data. The study included 425 eyes in 214 patients with a mean age of 32 ± 7.8 years. Mean spherical equivalent of the attempted correction (SE-ac) was -3.7 ± 1.7 diopters. Mean post-LASIK decrease in IOP was 4.6 ± 2.3 mmHg. The difference between preoperative and postoperative IOP was statistically significant (P < 0.001). SE-ac, preoperative IOP, and central corneal thickness had highly significant effects on postoperative IOP, based on linear regression analysis (P < 0.001 and R 2  = 0.043, P < 0.001 and R 2  = 0.370, and P < 0.001 and R 2  = 0.132, respectively). Regression model was created (F = 127.733, P < 0.001), and the adjusted R 2 value was 0.548. Evaluation of IOP after LASIK is important in myopic patients. The present study described a practical formula for predicting the true IOP with the aid of an IOP constant value in myopic eyes following LASIK.

DEMONSTRATION BULLETIN: IN SITU STEAM ENHANCED RECOVERY PROCESS - HUGHES ENVIRONMENTAL SYSTEMS, INC.

EPA Science Inventory

The Steam Enhanced Recovery Process (SERP) is designed to remove volatile compounds such as halogenated solvents and petroleum hydrocarbons, and semi-volatile compounds from contaminated soils in situ. The vapor pressures of most contaminants will increase by the addition of ste...

Comparison of in situ stratospheric ozone measurements obtained during the MAP/GLOBUS 1983 campaign

NASA Technical Reports Server (NTRS)

Aimedieu, P.; Matthews, W. A.; Attmannspacher, W.; Hartmannsgruber, R.; Cisneros, J.; Komhyr, W.; Robbins, D. E.

1987-01-01

Data from five types of in situ ozone sensors flown aboard ballons during the MAP/GLOBUS 1983 campaign were found to agree to within 5 percent uncertainty throughout the middle atmosphere. A description of the individual techniques and the error budget is given in addition to explanations for the discrepancies found at higher and lower altitudes. In comparison to UV photometry values, results from two electrochemical techniques were found to be greater in the lower atmosphere and to be lower in the upper atmosphere. In general, olefin chemiluminescence results were within 8 percent of the UV photometry results. Ozone column contents measured by the indigo colorization technique for two altitude regions of about 6 km height were greater than measurements from other techniques by 52 and 17 percent, respectively.

Comparison of in situ stratospheric ozone measurements obtained during the MAP/GLOBUS 1983 campaign

NASA Astrophysics Data System (ADS)

Aimedieu, P.; Matthews, W. A.; Attmannspacher, W.; Hartmannsgruber, R.; Cisneros, J.; Komhyr, W.; Robbins, D. E.

1987-05-01

Data from five types of in situ ozone sensors flown aboard ballons during the MAP/GLOBUS 1983 campaign were found to agree to within 5 percent uncertainty throughout the middle atmosphere. A description of the individual techniques and the error budget is given in addition to explanations for the discrepancies found at higher and lower altitudes. In comparison to UV photometry values, results from two electrochemical techniques were found to be greater in the lower atmosphere and to be lower in the upper atmosphere. In general, olefin chemiluminescence results were within 8 percent of the UV photometry results. Ozone column contents measured by the indigo colorization technique for two altitude regions of about 6 km height were greater than measurements from other techniques by 52 and 17 percent, respectively.

X-ray reflectivity measurements of liquid/solid interfaces under high hydrostatic pressure conditions.

PubMed

Wirkert, Florian J; Paulus, Michael; Nase, Julia; Möller, Johannes; Kujawski, Simon; Sternemann, Christian; Tolan, Metin

2014-01-01

A high-pressure cell for in situ X-ray reflectivity measurements of liquid/solid interfaces at hydrostatic pressures up to 500 MPa (5 kbar), a pressure regime that is particularly important for the study of protein unfolding, is presented. The original set-up of this hydrostatic high-pressure cell is discussed and its unique properties are demonstrated by the investigation of pressure-induced adsorption of the protein lysozyme onto hydrophobic silicon wafers. The presented results emphasize the enormous potential of X-ray reflectivity studies under high hydrostatic pressure conditions for the in situ investigation of adsorption phenomena in biological systems.

Pressure-induced coordination changes in alkali-germanate melts - An in situ spectroscopic investigation

NASA Technical Reports Server (NTRS)

Farber, Danial L.; Williams, Quentin

1992-01-01

The structure of liquid Na2Ge2O5-H2O, a silicate melt analog, has been studied with Raman spectroscopy to pressures of 2.2 gigapascals. Upon compression, a peak near more than 240 wavenumbers associated with octahedral GeO6 groups grows relative to a peak near 500 wavenumbers associated with tetrahedral GeO4 groups. This change corresponds to an increase in octahedral germanium in the liquid from near 0 percent at ambient pressures to more than 50 percent at a pressure of 2.2 gigapascals. Silicate liquids pausibly undergo similar coordination changes at depth in the earth. Such structural changes may generate decreases in the fusion slopes of silicates at high pressures as well as neutrally buoyant magmas within the transition zone of the earth's mantle.

Ionization pattern obtained in electrospray ionization or atmospheric pressure chemical ionization interfaces for authorized antidepressants in Romania

NASA Astrophysics Data System (ADS)

Grecu, Iulia; Ionicǎ, Mihai; Vlǎdescu, Marian; Truţǎ, Elena; Sultan, Carmen; Viscol, Oana; Horhotǎ, Luminiţa; Radu, Simona

2016-12-01

Antidepressants were found in 1950. In the 1990s there was a new generation of antidepressants. They act on the level of certain neurotransmitters extrasinpatic by its growth. After their mode of action antidepressants may be: SSRIs (Selective Serotonin Reuptake Inhibitors); (Serotonin-Norepinephrine Reuptake Inhibitors); SARIs (Serotonin Antagonist Reuptake Inhibitors); NRIs (Norepinephrine Reuptake Inhibitors); NDRIs (Norepinephrine-Dopamine Reuptake Inhibitors) NDRAs (Norepinephrine-Dopamine Releasing Agents); TCAs (Tricyclic Antidepressants); TeCAs (Tetracyclic Antidepressants); MAOIs (Monoamine Oxidase Inhibitors); agonist receptor 5-HT1A (5- hydroxytryptamine); antagonist receptor 5-HT2; SSREs (Selective Serotonin Reuptake Enhancers) and Sigma agonist receptor. To determine the presence of antidepressants in biological products, it has been used a system HPLC-MS (High Performance Liquid Chromatography - Mass Spectrometry) Varian 12001. The system is equipped with APCI (Atmospheric Pressure Chemical Ionization) or ESI (ElectroSpray Ionization) interface. To find antidepressants in unknown samples is necessary to recognize them after mass spectrum. Because the mass spectrum it is dependent on obtaining private parameters work of HPLC-MS system, and control interfaces, the mass spectra library was filled with the mass spectra of all approved antidepressants in Romania. The paper shows the mass spectra obtained in the HPLCMS system.

In situ gelling dorzolamide loaded chitosan nanoparticles for the treatment of glaucoma.

PubMed

Katiyar, Shefali; Pandit, Jayamanti; Mondal, Rabi S; Mishra, Anil K; Chuttani, Krishna; Aqil, Mohd; Ali, Asgar; Sultana, Yasmin

2014-02-15

The most important risk associated with glaucoma is the onset and progression of intraocular pressure. The objective of this study was to formulate in situ gel of chitosan nanoparticles to enhance the bioavailability and efficacy of dorzolamide in the glaucoma treatment. Optimized nanoparticles were spherical in shape (particle size: 164 nm) with a loading efficiency of 98.1%. The ex vivo release of the optimized in situ gel nanoparticle formulation showed a sustained drug release as compared to marketed formulation. The gamma scintigraphic study of prepared in situ nanoparticle gel showed good corneal retention compared to marketed formulation. HET-CAM assay of the prepared formulation scored 0.33 in 5 min which indicates the non-irritant property of the formulation. Thus in situ gel of dorzolamide hydrochloride loaded nanoparticles offers a more intensive treatment of glaucoma and a better patient compliance as it requires fewer applications per day compared to conventional eye drops. Copyright © 2013 Elsevier Ltd. All rights reserved.

Optimization and analysis of NF3 in situ chamber cleaning plasmas

NASA Astrophysics Data System (ADS)

Ji, Bing; Yang, James H.; Badowski, Peter R.; Karwacki, Eugene J.

2004-04-01

We report on the optimization and analysis of a dilute NF3 in situ plasma-enhanced chemical vapor deposition chamber cleaning plasma for an Applied Materials P-5000 DxL chamber. Using design of experiments methodology, we identified and optimized operating conditions within the following process space: 10-15 mol % NF3 diluted with helium, 200-400 sccm NF3 flow rate, 2.5-3.5 Torr chamber pressure, and 950 W rf power. Optical emission spectroscopy and Fourier transform infrared spectroscopy were used to endpoint the cleaning processes and to quantify plasma effluent emissions, respectively. The results demonstrate that dilute NF3-based in situ chamber cleaning can be a viable alternative to perfluorocarbon-based in situ cleans with added benefits. The relationship between chamber clean time and fluorine atom density in the plasma is also investigated.

Fast pressure-sensor system

NASA Technical Reports Server (NTRS)

Gross, C.

1976-01-01

Miniature silicon-diaphragm sensors and signal multiplexer are mounted to ganged zero-operate-calibrate pressure selector switches. Device allows in-situ calibration, can be computer controlled, and measures at approximately 10,000 readings per second.

Brucite [Mg(OH2)] Carbonation in Wet Supercritical CO2: An in situ High Pressure X-Ray Diffraction Study

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

Schaef, Herbert T.; Windisch, Charles F.; McGrail, B. Peter

2011-11-01

Understanding mechanisms and kinetics of mineral carbonation reactions relevant to sequestering carbon dioxide as a supercritical fluid (scCO2) in geologic formations is crucial to accurately predicting long-term storage risks. Most attention so far has been focused on reactions occurring between silicate minerals and rocks in the aqueous dominated CO2-bearing fluid. However, water-bearing scCO2 also comprises a reactive fluid, and in this situation mineral carbonation mechanisms are poorly understood. Using in situ high-pressure x-ray diffraction, the carbonation of brucite [Mg(OH)2] in wet scCO2 was examined at pressure (82 bar) as a function of water concentration and temperature (50 C and 75more » C). Exposing brucite to anhydrous scCO2 at either temperature resulted in little or no detectable reaction over three days. However, addition of trace amounts of water resulted in partial carbonation of brucite into nesquehonite [MgCO3 3H2O] within a few hours at 50 C. By increasing water content to well above the saturation level of the scCO2, complete conversion of brucite into nesquehonite was observed. Tests conducted at 75 C resulted in the conversion of brucite into magnesite [MgCO3] instead, apparently through an intermediate nesquehonite step. Raman spectroscopy applied to brucite reacted with 18O-labeled water in scCO2 show it was incorporated into carbonate at relatively high concentration. This supports a carbonation mechanism with at least one step involving a direct reaction between the mineral and water molecules without mediation by a condensed aqueous layer.« less

The ability of pulse pressure variations obtained with CNAP™ device to predict fluid responsiveness in the operating room.

PubMed

Biais, Matthieu; Stecken, Laurent; Ottolenghi, Laetitia; Roullet, Stéphanie; Quinart, Alice; Masson, Françoise; Sztark, François

2011-09-01

Respiratory-induced pulse pressure variations obtained with an arterial line (ΔPP(ART)) indicate fluid responsiveness in mechanically ventilated patients. The Infinity® CNAP™ SmartPod® (Dräger Medical AG & Co. KG, Lübeck, Germany) provides noninvasive continuous beat-to-beat arterial blood pressure measurements and a near real-time pressure waveform. We hypothesized that respiratory-induced pulse pressure variations obtained with the CNAP system (ΔPP(CNAP)) predict fluid responsiveness as well as ΔPP(ART) predicts fluid responsiveness in mechanically ventilated patients during general anesthesia. Thirty-five patients undergoing vascular surgery were studied after induction of general anesthesia. Stroke volume (SV) measured with the Vigileo™/FloTrac™ (Edwards Lifesciences, Irvine, CA), ΔPP(ART), and ΔPP(CNAP) were recorded before and after intravascular volume expansion (VE) (500 mL of 6% hydroxyethyl starch 130/0.4). Subjects were defined as responders if SV increased by ≥15% after VE. Twenty patients responded to VE and 15 did not. The correlation coefficient between ΔPP(ART) and ΔPP(CNAP) before VE was r = 0.90 (95% confidence interval [CI] = 0.84-0.96; P < 0.0001). Before VE, ΔPP(ART) and ΔPP(CNAP) were significantly higher in responders than in nonresponders (P < 0.0001). The values of ΔPP(ART) and ΔPP(CNAP) before VE were significantly correlated with the percent increase in SV induced by VE (respectively, r(2) = 0.50; P < 0.0001 and r(2) = 0.57; P < 0.0001). Before VE, a ΔPP(ART) >10% discriminated between responders and nonresponders with a sensitivity of 90% (95% CI = 69%-99%) and a specificity of 87% (95% CI = 60%-98%). The area under the receiver operating characteristic (ROC) curve was 0.957 ± 0.035 for ΔPP(ART). Before VE, a ΔPP(CNAP) >11% discriminated between responders and nonresponders with a sensitivity of 85% (95% CI = 62%-97%) and a specificity of 100% (95% CI = 78%-100%). The area under the ROC curve was 0.942 ± 0

XANES study on Fe, U and Th in hydrous melts at high temperature and pressure

NASA Astrophysics Data System (ADS)

Wilke, M.; Schmidt, C.; Farges, F.; Borchert, M.; Simionovici, A.; Hahn, M.

2005-12-01

Insight to the structural units of melts is an important key to model properties of magmas. The effect of water and pressure on the local structure around minor to trace elements in silicate melts was investigated at in-situ conditions. The study was performed using XANES spectroscopy and a diamond anvil-cell. This was done to characterize spurious effects observed on glasses that are potentially invoked by quenching [1] and to understand better the processes occurring during the quench. We present results of in-situ XANES measurements on iron, uranium and thorium in hydrous silicate melt up to 1 GPa and 700° C. In-situ XANES spectra were recorded at the ESRF (Grenoble, France), beamline ID 22, using a hydrothermal diamond anvil cell with a design optimized for such measurements [2], i.e. recesses on the front and the back-side of one of the diamond anvils that provide the possibility to collect spectra at relatively low energies (down to 7 keV) and relatively low concentrations (0.1-1 wt%). In-situ Fe K-edge XANES spectra of Fe(II) in hydrous haplogranitic melt at 700° C and 500 MPa suggests that the local structure around Fe in hydrous glass observed previously is probably due to ordering during the quench. Additionally, the XANES is very similar to in-situ spectra taken on Fe(II) in anhydrous haplogranitic melt at 1150° C and ambient pressure. This indicates that the combined effect of water and pressure (0-500 MPa range) does not influence drastically the local structure of Fe in this type of melt composition. In-situ LIII-edge XANES of U in hydrous haplogranitic melt (1 wt% U) at 700° C and 620 MPa show that, upon reduction, U precipitated as uraninite. This suggests a low amount of NBO's (to which tetravalent actinides preferentially bond [3]) in this water-saturated melt. In contrast, U-bearing (1000 ppm) hydrous sodium-tri-silicate melt shows the presence of U(IV) dissolved in the melt as 6-7 coordinated species, as in dry glasses [3]. Similar

In-situ pyrogenic production of biodiesel from swine fat.

PubMed

Lee, Jechan; Tsang, Yiu Fai; Jung, Jong-Min; Oh, Jeong-Ik; Kim, Hyung-Wook; Kwon, Eilhann E

2016-11-01

In-situ production of fatty acid methyl esters from swine fat via thermally induced pseudo-catalytic transesterification on silica was investigated in this study. Instead of methanol, dimethyl carbonate (DMC) was used as acyl acceptor to achieve environmental benefits and economic viability. Thermo-gravimetric analysis of swine fat reveals that swine fat contains 19.57wt.% of water and impurities. Moreover, the fatty acid profiles obtained under various conditions (extracted swine oil+methanol+NaOH, extracted swine oil+DMC+pseudo-catalytic, and swine fat+DMC+pseudo-catalytic) were compared. These profiles were identical, showing that the introduced in-situ transesterification is technically feasible. This also suggests that in-situ pseudo-catalytic transesterification has a high tolerance against impurities. This study also shows that FAME yield via in-situ pseudo-catalytic transesterification of swine fat reached up to 97.2% at 380°C. Therefore, in-situ pseudo-catalytic transesterification can be applicable to biodiesel production of other oil-bearing biomass feedstocks. Copyright © 2016 Elsevier Ltd. All rights reserved.

In-Situ Tuff Water Migration/Heater Experiment: posttest thermal analysis

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

Eaton, R.R.; Johnstone, J.K.; Nunziato, J.W.

This report describes posttest laboratory experiments and thermal computations for the In-Situ Tuff Water Migration/Heater Experiment that was conducted in Grouse Canyon Welded Tuff in G-Tunnel, Nevada Test Site. Posttest laboratory experiments were designed to determine the accuracy of the temperatures measured by the rockwall thermocouples during the in-situ test. The posttest laboratory experiments showed that the measured in-situ rockwall temperatures were 10 to 20{sup 0}C higher than the true rockwall temperatures. The posttest computational results, obtained with the thermal conduction code COYOTE, were compared with the experimentally obtained data and with calculated pretest results. Daily heater output power fluctuationsmore » (+-4%) caused by input power line variations and the sensitivity of temperature to heater output power required care in selecting the average heater output power values used in the code. The posttest calculated results compare reasonably well with the experimental data. 10 references, 14 figures, 5 tables.« less

AsS melt under pressure: one substance, three liquids.

PubMed

Brazhkin, V V; Katayama, Y; Kondrin, M V; Hattori, T; Lyapin, A G; Saitoh, H

2008-04-11

An in situ high-temperature--high-pressure study of liquid chalcogenide AsS by x-ray diffraction, resistivity measurements, and quenching from melt is presented. The obtained data provide direct evidence for the existence in the melt under compression of two transformations: one is from a moderate-viscosity molecular liquid to a high-viscosity nonmetallic polymerized liquid at P approximately 1.6-2.2 GPa; the other is from the latter to a low-viscosity metallic liquid at P approximately 4.6-4.8 GPa. Upon rapid cooling, molecular and metallic liquids crystallize to normal and high-pressure phases, respectively, while a polymerized liquid is easily quenched to a new AsS glass. General aspects of multiple phase transitions in liquid AsS, including relations to the phase diagram of the respective crystalline, are discussed.

In Situ Industrial Bimetallic Catalyst Characterization using Scanning Transmission Electron Microscopy and X-ray Absorption Spectroscopy at One Atmosphere and Elevated Temperature.

PubMed

Prestat, Eric; Kulzick, Matthew A; Dietrich, Paul J; Smith, Mr Matthew; Tien, Mr Eu-Pin; Burke, M Grace; Haigh, Sarah J; Zaluzec, Nestor J

2017-08-18

We have developed a new experimental platform for in situ scanning transmission electron microscope (STEM) energy dispersive X-ray spectroscopy (EDS) which allows real time, nanoscale, elemental and structural changes to be studied at elevated temperature (up to 1000 °C) and pressure (up to 1 atm). Here we demonstrate the first application of this approach to understand complex structural changes occurring during reduction of a bimetallic catalyst, PdCu supported on TiO 2 , synthesized by wet impregnation. We reveal a heterogeneous evolution of nanoparticle size, distribution, and composition with large differences in reduction behavior for the two metals. We show that the data obtained is complementary to in situ STEM electron energy loss spectroscopy (EELS) and when combined with in situ X-ray absorption spectroscopy (XAS) allows correlation of bulk chemical state with nanoscale changes in elemental distribution during reduction, facilitating new understanding of the catalytic behavior for this important class of materials. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results

Effect of Processing Pressure on Isolated Pore Formation during Controlled Directional Solidification in Small Channels

NASA Technical Reports Server (NTRS)

Cox, Matthew C.; Anilkumar, Amrutur V.; Grugel, RIchard N.; Lee, Chun P.

2008-01-01

Directional solidification experiments were performed, using succinonitrile saturated with nitrogen gas, to examine the effects of in-situ processing pressure changes on the formation growth, and evolution of an isolated, cylindrical gaseous pore. A novel solidification facility, capable of processing thin cylindrical samples (I.D. < 1.0 mm), under controlled pressure conditions, was used for the experiments. A new experimental method for growing the isolated pore from a seed bubble is introduced. The experimental results indicate that an in-situ processing pressure change will result in either a transient change in pore diameter or a complete termination of pore growth, indicating that pressure changes can be used as a control parameter to terminate bubble growth. A simple analytical model has been introduced to explain the experimental observations.

In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

DOE PAGES

Ferrari, S.; Kumar, R. S.; Grinblat, F.; ...

2016-04-23

We have studied the high-pressure structural behavior of zinc ferrite (ZnFe 2O 4) nanoparticles by powder X-ray diffraction measurements up to 47 GPa. We found that the cubic spinel structure of ZnFe 2O 4 remains up to 33 GPa and a phase transition is induced beyond this pressure. The high-pressure phase is indexed to an orthorhombic CaMn 2O 4-type structure. Upon decompression the low- and high-pressure phases coexist. The compressibility of both structures was also investigated. We have observed that the lattice parameters of the high-pressure phase behave anisotropically upon compression. Further, we predict possible phase transition around 55 GPa.more » For comparison, we also studied the compression behavior of magnetite (Fe 3O 4) nanoparticles by X-ray diffraction up to 23 GPa. Spinel-type ZnFe 2O 4 and Fe 3O 4 nanoparticles have a bulk modulus of 172 (20) GPa and 152 (9) GPa, respectively. Lastly, this indicates that in both cases the nanoparticles do not undergo a Hall-Petch strengthening.« less

In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

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

Ferrari, S.; Kumar, R. S.; Grinblat, F.

We have studied the high-pressure structural behavior of zinc ferrite (ZnFe 2O 4) nanoparticles by powder X-ray diffraction measurements up to 47 GPa. We found that the cubic spinel structure of ZnFe 2O 4 remains up to 33 GPa and a phase transition is induced beyond this pressure. The high-pressure phase is indexed to an orthorhombic CaMn 2O 4-type structure. Upon decompression the low- and high-pressure phases coexist. The compressibility of both structures was also investigated. We have observed that the lattice parameters of the high-pressure phase behave anisotropically upon compression. Further, we predict possible phase transition around 55 GPa.more » For comparison, we also studied the compression behavior of magnetite (Fe 3O 4) nanoparticles by X-ray diffraction up to 23 GPa. Spinel-type ZnFe 2O 4 and Fe 3O 4 nanoparticles have a bulk modulus of 172 (20) GPa and 152 (9) GPa, respectively. Lastly, this indicates that in both cases the nanoparticles do not undergo a Hall-Petch strengthening.« less

Modeling of Permeability Structure Using Pore Pressure and Borehole Strain Monitoring

NASA Astrophysics Data System (ADS)

Kano, Y.; Ito, H.

2011-12-01

Hydraulic or transport property, especially permeability, of the rock affect the behavior of the fault during earthquake rupture and also interseismic period. The methods to determine permeability underground are hydraulic test utilizing borehole and packer or core measurement in laboratory. Another way to know the permeability around a borehole is to examine responses of pore pressure to natural loading such as barometric pressure change at surface or earth tides. Using response to natural deformation is conventional method for water resource research. The scale of measurement is different among in-situ hydraulic test, response method, and core measurement. It is not clear that the relationship between permeability values form each method for an inhomogeneous medium such as a fault zone. Supposing the measurement of the response to natural loading, we made a model calculation of permeability structure around a fault zone. The model is 2 dimensional and constructed with vertical high-permeability layer in uniform low-permeability zone. We assume the upper and lower boundaries are drained and no-flow condition. We calculated the flow and deformation of the model for step and cyclic loading by numerically solving a two-dimensional diffusion equation. The model calculation shows that the width of the high-permeability zone and contrast of the permeability between high- and low- permeability zones control the contribution of the low-permeability zone. We made a calculation with combinations of permeability and fault width to evaluate the sensitivity of the parameters to in-situ measurement of permeability. We applied the model calculation to the field results of in-situ packer test, and natural response of water level and strain monitoring carried out in the Kamioka mine. The model calculation shows that knowledge of permeability in host rock is also important to obtain permeability of fault zone itself. The model calculations help to design long-term pore pressure

A highly sensitive in-situ turbidity sensor with low power consumption

NASA Astrophysics Data System (ADS)

Hu, Yi; Sun, Lei; Ye, Shuming; Chen, Hang; Jiang, Kai; Pan, Jianming

2014-03-01

A highly sensitive in-situ turbidity sensor with the low power consumption was proposed and evaluated in this study. To meet the practical requirements of the in-situ detection, we have designed the light scattering path, watertight mechanical structure, and ultra-weak scattering light detecting method. Experiments showed that the sensor had a sensitivity of 0.0076 FTU with the concentration range of 0-25 FTU and the R-square of 0.9999. The sensor could withstand the water pressure in depth of 1000 m and had the low power consumption in the active mode 10.4 mA, sleep mode 65 μA with a supply voltage of 8.4 V. Southern China Sea buoy experiments indicated that the sensor could work well in the actual in-situ environment. In comparison with sensors of other companies, our sensor had relatively more comprehensive performance.

Dust Removal Technolgy for a Mars In Situ Resource Utilization System

NASA Technical Reports Server (NTRS)

Calle, C. I.; Johansen, M. R.; Williams, B. S.; Hogue, M. D.; Mackey, P. J.; Clements, J. S.

2011-01-01

Several In Situ Resource Utilization (lSRU) systems being considered to enable future manned exploration of Mars require capture of Martian atmospheric gas to extract oxygen and other commodities. However, the Martian atmosphere contains relatively large amounts of dust which must be removed in tbe collection systems of the ISRU chambers. The amount of atmospheric dust varies largely with the presence of daily dust devils and the less frequent but much more powerful global dust storms. A common and mature dust removal technology for terrestrial systems is the electrostatic precipitator. With this technology, dust particles being captured are imparted an electrostatic charge by means of a corona discharge. Charged dust particles are then driven to a region of high electric field which forces the particles onto a collector for capture. Several difficulties appear when this technology is adapted to the Martian atmospheric environment At the low atmospheric pressure of Mars, electrical breakdown occurs at much lower voltages than on Earth and corona discharge is difficult to sustain. In this paper, we report on our efforts to obtain a steady corona/glow discharge in a simulated Martian atmosphere of carbon dioxide at 9 millibars of pressure. We also present results on the design of a dust capture system under these atmospheric conditions.

Localised corrosion in aluminium alloy 2024-T3 using in situ TEM.

PubMed

Malladi, Sairam; Shen, Chenggang; Xu, Qiang; de Kruijff, Tom; Yücelen, Emrah; Tichelaar, Frans; Zandbergen, Henny

2013-11-28

An approach to carry out chemical reactions using aggressive gases in situ in a transmission electron microscope (TEM), at ambient pressures of 1.5 bar using a windowed environmental cell, called a nanoreactor, is presented here. The nanoreactor coupled with a specially developed holder with platinum tubing permits the usage of aggressive chemicals like hydrochloric acid (HCl).

In Situ Observation of High-Pressure Phase Transitions in SiO2 Under Shock Loading Using Time Resolved X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Tracy, S. J.; Turneaure, S.; Duffy, T. S.

2016-12-01

Quartz is one of the most abundant minerals in Earth's crust and serves as an archetype for silicate minerals generally. The shock metamorphism of silica is important for understanding and interpreting meteorite impact events. Shock compression of quartz is characterized by a phase transition occurring over a broad mixed-phase region ( 10-40 GPa). Despite decades of study, the nature of this transformation and the structure of the high-pressure phase remain poorly understood. In situ x-ray diffraction data on shock-compressed SiO2 was collected at the Dynamic Compression Sector at the Advanced Photon Source. The behavior both single crystal alpha-quartz and fused silica was investigated under dynamic loading through a series real-time synchrotron x-ray diffraction measurements during peak stresses up to 65 GPa. A two-stage light gas gun was used to accelerate LiF flyer plates that impacted the SiO2 samples resulting in a propagating step-like increase in pressure and temperature behind the shock front. Four consecutive x-ray frames, separated by 153 ns, were collected during the transient loading and unloading. These measurements allow for the determination of time-dependent atomic arrangements, demonstrating that both amorphous silica as well as crystalline alpha-quartz transform to stishovite above 36 GPa. These measurements reveal important information about the role of kinetics as well texture development and potential defect structures in the transformed material.

Water Pressure Effects on Strength and Deformability of Fractured Rocks Under Low Confining Pressures

NASA Astrophysics Data System (ADS)

Noorian Bidgoli, Majid; Jing, Lanru

2015-05-01

The effect of groundwater on strength and deformation behavior of fractured crystalline rocks is one of the important issues for design, performance and safety assessments of surface and subsurface rock engineering problems. However, practical difficulties make the direct in situ and laboratory measurements of these properties of fractured rocks impossible at present, since effects of complex fracture system hidden inside the rock masses cannot be accurately estimated. Therefore, numerical modeling needs to be applied. The overall objective of this paper is to deepen our understanding on the validity of the effective stress concept, and to evaluate the effects of water pressure on strength and deformation parameters. The approach adopted uses discrete element methods to simulate the coupled stress-deformation-flow processes in a fractured rock mass with model dimensions at a representative elementary volume (REV) size and realistic representation of fracture system geometry. The obtained numerical results demonstrate that water pressure has significant influence on the strength, but with minor effects on elastic deformation parameters, compared with significant influence by the lateral confining pressure. Also, the classical effective stress concept to fractured rock can be quite different with that applied in soil mechanics. Therefore, one should be cautious when applying the classical effective stress concept to fractured rock media.

Monitoring Nanoparticle Synthesis in a Carbon Arc Discharge Environment, In Situ

NASA Astrophysics Data System (ADS)

Mitrani, James

This work presents experimental and theoretical studies of gas-phase synthesis of fullerenes and carbon nanoparticles in the presence of an atmospheric-pressure, arc discharge plasma. Carbon arc discharges have been used for synthesizing carbon nanotubes for over 25 years, and have the potential for economically synthesizing industrial-scale quantities of fullerenes. However, the efficiency and selectivity of fullerene synthesis with carbon arc discharges are quite low. Optimizing carbon arc discharges for fullerene synthesis requires a thorough understanding of the dynamics behind gas-phase nanoparticle synthesis in the presence of an arc discharge plasma. We built a carbon arc discharge setup to study nanoparticle and fullerene synthesis. The laser-induced incandescence (LII) diagnostic was applied for monitoring nanoparticle synthesis, in situ. The LII diagnostic had previously been applied as a combustion diagnostic for in situ measurements of concentrations and sizes of soot particles in flame environments. Prior to the present study, it had never been applied for studying fullerenes, nor had it been applied to study nanoparticles in the presence of an atmospheric-pressure plasma. Therefore, experiments were designed that allowed for the calibration of the LII diagnostic with research-grade, arc-synthesized soot particles and carbon nanotubes. Additionally, the theory and models underpinning the LII diagnostic were adapted to include the presence of an atmospheric-pressure, arc-discharge plasma. Results presented in this work confirm the ability of the LII diagnostic to measure sizes of arc-synthesized nanoparticles in situ, and show the spatial location of high densities of arc-synthesized nanoparticles with respect to the arc discharge plasma. Determining the spatial location of nanoparticle synthesis and growth is crucial for understanding the background conditions (e.g. background gas temperature, electron densities ...) in which nanoparticles nucleate and

Sub-Kelvin magnetic and electrical measurements in a diamond anvil cell with in situ tunability

NASA Astrophysics Data System (ADS)

Palmer, A.; Silevitch, D. M.; Feng, Yejun; Wang, Yishu; Jaramillo, R.; Banerjee, A.; Ren, Y.; Rosenbaum, T. F.

2015-09-01

We discuss techniques for performing continuous measurements across a wide range of pressure-field-temperature phase space, combining the milli-Kelvin temperatures of a helium dilution refrigerator with the giga-Pascal pressures of a diamond anvil cell and the Tesla magnetic fields of a superconducting magnet. With a view towards minimizing remnant magnetic fields and background magnetic susceptibility, we characterize high-strength superalloy materials for the pressure cell assembly, which allows high fidelity measurements of low-field phenomena such as superconductivity below 100 mK at pressures above 10 GPa. In situ tunability and measurement of the pressure permit experiments over a wide range of pressure, while at the same time making possible precise steps across abrupt phase transitions such as those from insulator to metal.

Mass-induced sea level variations in the Red Sea from steric-corrected altimetry, GRACE, in-situ bottom pressure records, and hydrographic observations

NASA Astrophysics Data System (ADS)

Feng, Wei; Lemoine, Jean-Michel; Zhong, Min; Xu, Houze

2014-05-01

An annual amplitude of ~18 cm mass-induced sea level variations (SLV) in the Red Sea is detected from steric-corrected altimetry and the Gravity Recovery and Climate Experiment (GRACE) satellites from 2003 to 2011, which dominates the mean sea level in the region. Seawater mass variations here generally reach maximum in late January/early February. The steric component of SLV calculated from oceanographic temperature and salinity data is relatively small and peaks about seven months later than mass variations. The phase difference between the steric SLV and the mass-induced SLV indicates that when the Red Sea gains the mass from inflow water in winter, the steric SLV fall, and vice versa in summer. In-situ bottom pressure records in the eastern coast of the Red Sea validate the high mass variability observed by steric-corrected altimetry and GRACE. Furthermore, we compare the horizontal water mass flux in the Red Sea from steric-corrected altimetry and GRACE with that estimated from hydrographic observations.

In situ chemical osmosis experiment in the Boom Clay at the Mol underground research laboratory

NASA Astrophysics Data System (ADS)

Garavito, A. M.; De Cannière, P.; Kooi, H.

Studies on the compatibility of Boom Clay with large amounts of nitrate- bearing bituminized radioactive waste have recently raised a particular interest for osmosis-induced effects in this reference formation in Belgium. Indeed, water flow and solute transport may be associated with several types of driving forces, or gradients (chemical, electrical, thermal), in addition to the hydraulic forces, resulting in the so-called coupled flows. Fluid flow caused by driving forces different than hydraulic gradients is referred to as osmosis. Chemical osmosis, the water flow induced by a chemical gradient across a semi-permeable membrane, can generate pressure increase. The question thus arises if there is a risk to create high pore pressures that could damage the near-field of medium-level waste (MLW) galleries, if osmotically driven water flows towards the galleries are produced by the release of large amounts of NaNO 3 (750 t) in the formation. To what extent a low-permeability clay formation such as the Boom Clay acts as an osmotic membrane is thus a key issue to assess the relevance of osmosis phenomena for the disposal of medium-level waste. An in situ osmosis experiment has been conducted at the H ADES underground research laboratory to determine the osmotic efficiency of Boom Clay at the field scale. A recently developed chemical osmosis flow continuum model has been used to design the osmosis experiment, and to interpret the water pressure measurements. Experimental data could be reproduced quite accurately by the model, and the inferred parameter values are consistent with independent determinations for Boom Clay. A rapid water pressure increase (but limited to about a 2 m water column) was observed after 12 h in the filter containing the more saline water. Then, the osmotically induced water pressure slowly decays on several months. So, the experimental results obtained in situ confirm the occurrence of non-hydraulic flow phenomena (chemical osmosis) in a low

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.

Ion funnel augmented Mars atmospheric pressure photoionization mass spectrometry for in situ detection of organic molecules.

PubMed

Johnson, Paul V; Hodyss, Robert; Beauchamp, J L

2014-11-01

Laser desorption is an attractive technique for in situ sampling of organics on Mars given its relative simplicity. We demonstrate that under simulated Martian conditions (~2.5 Torr CO(2)) laser desorption of neutral species (e.g., polycyclic aromatic hydrocarbons), followed by ionization with a simple ultraviolet light source such as a discharge lamp, offers an effective means of sampling organics for detection and identification with a mass spectrometer. An electrodynamic ion funnel is employed to provide efficient ion collection in the ambient Martian environment. This experimental methodology enables in situ sampling of Martian organics with minimal complexity and maximum flexibility.

High-pressure hydrogen respiration in hydrothermal vent samples from the deep biosphere

NASA Astrophysics Data System (ADS)

Morgan-Smith, D.; Schrenk, M. O.

2013-12-01

Cultivation of organisms from the deep biosphere has met with many challenges, chief among them the ability to replicate this extreme environment in a laboratory setting. The maintenance of in situ pressure levels, carbon sources, and gas concentrations are important, intertwined factors which may all affect the growth of subsurface microorganisms. Hydrogen in particular is of great importance in hydrothermal systems, but in situ hydrogen concentrations are largely disregarded in attempts to culture from these sites. Using modified Hungate-type culture tubes (Bowles et al. 2011) within pressure-retaining vessels, which allow for the dissolution of higher concentrations of gas than is possible with other culturing methods, we have incubated hydrothermal chimney and hydrothermally-altered rock samples from the Lost City and Mid-Cayman Rise hydrothermal vent fields. Hydrogen concentrations up to 15 mmol/kg have been reported from Lost City (Kelley et al. 2005), but data are not yet available from the recently-discovered Mid-Cayman site, and the elevated concentration of 30 mmol/kg is being used in all incubations. We are using a variety of media types to enrich for various metabolic pathways including iron and sulfur reduction under anoxic or microaerophilic conditions. Incubations are being carried out at atmospheric (0.1 MPa), in situ (9, 23, or 50 MPa, depending on site), and elevated (50 MPa) pressure levels. Microbial cell concentrations, taxonomic diversity, and metabolic activities are being monitored during the course of these experiments. These experiments will provide insight into the relationships between microbial activities, pressure, and gas concentrations typical of deep biosphere environments. Results will inform further culturing studies from both fresh and archived samples. References cited: Bowles, M.W., Samarkin, V.A., Joye, S.B. 2011. Improved measurement of microbial activity in deep-sea sediments at in situ pressure and methane concentration

Correlation between structural change and electrical transport properties of Fe-doped chrysotile nanotubes under high pressure

NASA Astrophysics Data System (ADS)

Zhang, Junkai; Yang, Lili; Wu, Xiaoxin; Wei, Maobin; Liu, Yanqing; Gao, Chunxiao; Yang, Jinghai; Ma, Yanzhang

2018-04-01

Fe3+ doped chrysotile nanotubes (NTs) have been synthesized under controlled hydrothermal conditions, and have been characteristic of layered-walls and room-temperature ferromagnetism. High-pressure in situ impedance spectra and synchrotron XRD measurements are performed on Fe-doped chrysotile NTs to reveal the electrical transport and structural properties under compression. Sample resistance (R sum) was found to increase with the pressure elevation, accompanying the step decrease in the grain boundary relaxation frequency (f gb), which reflects the bandgap broadening and dipoles polarization weakening due to the application of pressure. Furthermore, it is found that both R sum and f gb change their pressure dependences at ~5.0 GPa, which is attributed to the nonlinear compressibility of c-axis and even the underlying lattice distortion of monoclinic structure obtained in the XRD observations.

A Reactive Oxide Overlayer on Rh Nanoparticles during CO Oxidation and Its Size Dependence Studied by in Situ Ambient Pressure XPS

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

Grass, Michael E.; Zhang, Yawen; Butcher, Derek R.

2008-09-15

CO oxidation is one of the most studied heterogeneous reactions, being scientifically and industrially important, particularly for removal of CO from exhaust streams and preferential oxidation for hydrogen purification in fuel cell applications. The precious metals Ru, Rh, Pd, Pt, and Au are most commonly used for this reaction because of their high activity and stability. Despite the wealth of experimental and theoretical data, it remains unclear what is the active surface for CO oxidation under catalytic conditions for these metals. In this communication, we utilize in situ synchrotron ambient pressure X-ray photoelectron spectroscopy (APXPS) to monitor the oxidation statemore » at the surface of Rh nanoparticles during CO oxidation and demonstrate that the active catalyst is a surface oxide, the formation of which is dependent on particle size. The amount of oxide formed and the reaction rate both increase with decreasing particle size.« less

Pressure balance cross-calibration method using a pressure transducer as transfer standard

PubMed Central

Olson, D; Driver, R. G.; Yang, Y

2016-01-01

Piston gauges or pressure balances are widely used to realize the SI unit of pressure, the pascal, and to calibrate pressure sensing devices. However, their calibration is time consuming and requires a lot of technical expertise. In this paper, we propose an alternate method of performing a piston gauge cross calibration that incorporates a pressure transducer as an immediate in-situ transfer standard. For a sufficiently linear transducer, the requirement to exactly balance the weights on the two pressure gauges under consideration is greatly relaxed. Our results indicate that this method can be employed without a significant increase in measurement uncertainty. Indeed, in the test case explored here, our results agreed with the traditional method within standard uncertainty, which was less than 6 parts per million. PMID:28303167

Pressure-induced anomalies and structural instability in compressed β-Sb 2 O 3

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

Zou, Yongtao; Zhang, Wei; Li, Xuefei

2018-01-01

Here, we have discovered a new high-pressure phase of Sb 2 O 3 , and reported pressure-induced anomalies in orthorhombic β-Sb 2 O 3 (valentinite) by the combination of synchrotron in situ X-ray diffraction and first-principles theoretical calculations up to 40.5 GPa.

Effect of hydrogen pressure on free radicals in direct coal liquefaction/coprocessing

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

Seehra, M.S.; Ibrahim, M.M.

1995-12-31

The objective of this study was to investigate the coprocessing of coal with waste tires and commingled plastics and to characterize the relevant catalysts, using high pressure/high temperature in-situ ESR (Electron Spin Resonance) spectroscopy. The recent results from high pressure ESR spectroscopy are emphasized. During this period, considerable progress was made in developing the high pressure capabilities in in-situ ESR spectroscopy and new results carried out in 1000 psi of H{sub 2}gas are presented. In these experiments, sapphire tubes were used to contain the high pressures at temperatures up to 500{degrees}C. Results of the experiments carried out under 1000 psimore » of H{sub 2} are compared with those under 1000 psi of non-interacting argon and with the earlier experiments in flowing H{sub 2} gas where the volatiles are removed by the flowing gas. In these experiments, the free radical density N of the Blind Canyon coal was measured at each temperature and pressure by double integration of the ESR signal and calibrating it against a standard. The details of the experimental apparatus and procedures have been described in earlier publications.« less

Crystallization of TiO2 Nanotubes by In Situ Heating TEM

PubMed Central

Casu, Alberto; Lamberti, Andrea

2018-01-01

The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy. PMID:29342894

In-Situ Leak Testing And Replacement Of Glovebox Isolator, Or Containment Unit Gloves

DOEpatents

Castro, Julio M.; Macdonald, John M.; Steckle, Jr., Warren P.

2004-11-02

A test plug for in-situ testing a glove installed in a glovebox is provided that uses a top plate and a base plate, and a diametrically expandable sealing mechanism fitting between the two plates. The sealing mechanism engages the base plate to diametrically expand when the variable distance between the top plate and the bottom plate is reduced. An inlet valve included on the top plate is used to introducing a pressurized gas to the interior of the glove, and a pressure gauge located on the top plate is used to monitor the interior glove pressure.

The use of an optical method to evaluate prokaryotic oxygen consumption under high pressure condition

NASA Astrophysics Data System (ADS)

Garel, M.; Martini, S.; Lefèvre, D.; Tamburini, C.

2016-02-01

The heterotrophic prokaryotes are the main contributor to organic matter degradation in the ocean and particularly in the deep ocean. Nowadays, a classical way to evaluate the prokaryotic carbon demand (PCD) needs the estimation of both prokaryotic heterotrophic production (PHP) and prokaryotic respiration (PR). PHP measurements in deep-sea waters are relatively well documented and the importance of maintaining the in situ conditions (pressure and temperature) to avoid bias of the real deep-sea activities has been highlighted. However, no accurate methodology is available to measure directly, under in situ conditions (pressure and temperature) PR in the dark ocean. This study is presenting PR measurements under in situ conditions. High-pressure bottles have been adapted with a non-invasive sensor to measure prokaryotic oxygen consumption. The methodology is based on fluorescence quenching where molecular oxygen quenches the luminescence of planar-optode-oxygen sensor widely used in oceanography. Firstly, accuracy, detection limit, precision and response time of oxygen concentration measurements have been investigated in relation to an increase of hydrostatic pressure. Secondly, we will present experiments performed on natural prokaryotic consortium mixed with freshly collected particles to assess the O2 consumption in relation with increasing hydrostatic pressure (150 m depth per day). Finally, first results of coupled PHP and PR measurements at in situ conditions (temperature and pressure) from mesopelagic and bathypelagic samples of the Atlantic Ocean (PAP site), will be discussed. Finally, we will discuss first results of coupled PHP and PR measurements at in situ conditions (temperature and pressure) from Atlantic Ocean mesopelagic and bathypelagic samples (PAP site).

Synchrotron in-situ deformation experiments of perovskite + (Mg,Fe)O aggregates under shallow lower mantle conditions (Invited)

NASA Astrophysics Data System (ADS)

Girard, J.; Amulele, G.; Farla, R. J.; Liu, Z.; Mohiuddin, A.; Karato, S.

2013-12-01

Experimental studies on rheological properties of mantle's minerals are crucial to understand the dynamics of Earth's interior, but direct experimental studies under the relevant lower mantle conditions are challenging. Most of the earlier studies were performed at lower mantle pressures but low temperatures using DAC (diamond anvil cell) (e.g., Merkel et al., 2003)), and in DAC experiments strain-rate and stress are unknown. Some previous studies were carried out under high pressures and high temperatures (e.g, Cordier et al., 2004) , but quantitative results on rheological behaviour of said minerals were not obtained. Here we present the results of the first in-situ deformation experiments of perovskite + (Mg,Fe)O (Pv + fp) aggregates using RDA (rotational Drickamer apparatus). The RDA has a better support for the anvils at high pressure than the more commonly used D-DIA apparatus and hence we can reach higher pressures and temperatures than the D-DIA. We have recently made new modifications to the cell assembly to reach the lower mantle conditions with less interference in X-ray diffraction patterns by the surrounding materials. The starting material was ringwoodite synthesized using a multi-anvil. In-situ deformation experiments were then carried at pressure up to 28 GPa (calculated from thermal EOS of Pt) and estimated temperatures up to 2200 K using RDA. Under these conditions, ringwoodite transformed to Pv + fp. We subsequently deformed the sample between strain rates of 10-4 to 10-5 s-1. Stress and strain were measured in-situ using X-ray synchrotron beam. The recovered sample analyses show evidence of perovskite+(Mg,Fe)O microstructure (Fig. 1). The radial X-ray diffraction data are being analysed to determine the stress levels of two minerals. Also microstructures of deformed specimens are studied to understand the deformation mechanisms and strain partitioning. The results will contribute towards our understanding of the rheological properties of the

Optical properties of highly n-doped germanium obtained by in situ doping and laser annealing

NASA Astrophysics Data System (ADS)

Frigerio, J.; Ballabio, A.; Gallacher, K.; Giliberti, V.; Baldassarre, L.; Millar, R.; Milazzo, R.; Maiolo, L.; Minotti, A.; Bottegoni, F.; Biagioni, P.; Paul, D.; Ortolani, M.; Pecora, A.; Napolitani, E.; Isella, G.

2017-11-01

High n-type doping in germanium is essential for many electronic and optoelectronic applications especially for high performance Ohmic contacts, lasing and mid-infrared plasmonics. We report on the combination of in situ doping and excimer laser annealing to improve the activation of phosphorous in germanium. An activated n-doping concentration of 8.8  ×  1019 cm-3 has been achieved starting from an incorporated phosphorous concentration of 1.1  ×  1020 cm-3. Infrared reflectivity data fitted with a multi-layer Drude model indicate good uniformity over a 350 nm thick layer. Photoluminescence demonstrates clear bandgap narrowing and an increased ratio of direct to indirect bandgap emission confirming the high doping densities achieved.

In situ study at high pressure and temperature of the environment of water in hydrous Na and Ca aluminosilicate melts and coexisting aqueous fluids

NASA Astrophysics Data System (ADS)

Le Losq, Charles; Dalou, Célia; Mysen, Bjorn O.

2017-07-01

The bonding and speciation of water dissolved in Na silicate and Na and Ca aluminosilicate melts were inferred from in situ Raman spectroscopy of the samples, in hydrothermal diamond anvil cells, while at crustal temperature and pressure conditions. Raman data were also acquired on Na silicate and Na and Ca aluminosilicate glasses, quenched from hydrous melts equilibrated at high temperature and pressure in a piston cylinder apparatus. In the hydrous melts, temperature strongly influences O-H stretching ν(O-H) signals, reflecting its control on the bonding of protons between different molecular complexes. Pressure and melt composition effects are much smaller and difficult to discriminate with the present data. However, the chemical composition of the melt + fluid system influences the differences between the ν(O-H) signals from the melts and the fluids and, hence, between their hydrogen partition functions. Quenching modifies the O-H stretching signals: strong hydrogen bonds form in the glasses below the glass transition temperature Tg, and this phenomenon depends on glass composition. Therefore, glasses do not necessarily record the O-H stretching signal shape in melts near Tg. The melt hydrogen partition function thus cannot be assessed with certainty using O-H stretching vibration data from glasses. From the present results, the ratio of the hydrogen partition functions of hydrous silicate melts and aqueous fluids mostly depends on temperature and the bulk melt + fluid system chemical composition. This implies that the fractionation of hydrogen isotopes between magmas and aqueous fluids in water-saturated magmatic systems with differences in temperature and bulk chemical composition will be different.

Zeeman Effect in Ruby at High Pressures

NASA Astrophysics Data System (ADS)

Dan, Ioana

2012-02-01

We have developed a versatile fiber-coupled system for magneto-optical spectroscopy measurements at high pressure. The system is based on a miniature Cu-alloy Diamond Anvil Cell (from D'Anvils, Ltd) fitted with a custom-designed He gas-actuated membrane for in-situ pressure control, and coupled with a He transfer cryostat incorporating a superconducting magnet (from Quantum Designs). This system allows optical measurements (Raman, photoluminescence, reflectivity) within wide ranges of pressures (up to 100GPa), temperatures (4.2-300K) and magnetic fields (0-9T). We employ this system to examine the effect of pressure and non-hydrostatic stress on the Zeeman split d-d transitions of Cr^3+ in ruby (Al2O3: Cr^3+). We determine the effect of pressure and non-hydrostaticity on the trigonal crystal field in this material, and discuss the use of the Zeman-split ruby fluorescence as a possible probe for deviatoric stresses in diamond anvil cell experiments.

In-situ TEM on (de)hydrogenation of Pd at 0.5-4.5 bar hydrogen pressure and 20-400°C.

PubMed

Yokosawa, Tadahiro; Alan, Tuncay; Pandraud, Gregory; Dam, Bernard; Zandbergen, Henny

2012-01-01

We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 4.5 bar. The Pd film consisted of islands being 15 nm thick and 50-500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10-16°C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5-4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale. Copyright © 2011 Elsevier B.V. All rights reserved.

Nonoperative measurement of pancreatic and common bile duct pressures with a microtransducer catheter and effects of duodenoscopic sphincterotomy.

PubMed

Tanaka, M; Ikeda, S; Nakayama, F

1981-06-01

Duodenoscopic manometry of the pancreatic duct (PD) and common bile duct (CBD) using a microtransducer catheter was distinct advantages over infusion manometry, giving absolute values of in situ intraluminal pressure. Microtransducer manometry was performed without medication in 49 patients with gallbladder stones (10), common bile duct stones (24), hepatic duct stones (6) and common bile duct dilatation (9), and was successful in 42 (86%) for PD and 36 (73%) for CBD. Ductal pressures showed respiration-synchronized biphasic variations superimposed by the arterial pulsation effect. Considerable postural change of the pressure values suggested that the recording posture should be predetermined. The PD-to-duodenum pressure gradient was higher than the CBD-to-duodenum gradient in most cases. Both were lower than those obtained previously by infusion methods. No significant differences were found in pressure profiles of the four disease groups. Endoscopic sphincterotomy significantly reduced not only CBD pressure but also PD pressure.

Cooling of in-situ propellant rocket engines for Mars mission. M.S. Thesis - Cleveland State Univ.

NASA Technical Reports Server (NTRS)

Armstrong, Elizabeth S.

1991-01-01

One propulsion option of a Mars ascent/descent vehicle is multiple high-pressure, pump-fed rocket engines using in-situ propellants, which have been derived from substances available on the Martian surface. The chosen in-situ propellant combination for this analysis is carbon monoxide as the fuel and oxygen as the oxidizer. Both could be extracted from carbon dioxide, which makes up 96 percent of the Martian atmosphere. A pump-fed rocket engine allows for higher chamber pressure than a pressure-fed engine, which in turn results in higher thrust and in higher heat flux in the combustion chamber. The heat flowing through the wall cannot be sufficiently dissipated by radiation cooling and, therefore, a regenerative coolant may be necessary to avoid melting the rocket engine. The two possible fluids for this coolant scheme, carbon monoxide and oxygen, are compared analytically. To determine their heat transfer capability, they are evaluated based upon their heat transfer and fluid flow characteristics.

In situ detection of tropospheric OH and HO2 by laser-induced fluorescence in a detection chamber at low pressure

NASA Technical Reports Server (NTRS)

Brune, William H.; Stevens, Philip S.; Mather, James

1994-01-01

Just as in the method of Hard and O'Brien, ambient air is pulled through an approximately 1 mm diameter inlet into a detection chamber that is maintained at a pressure of 2.4 torr. The ambient air stream travels through the detection chamber with a velocity of greater than 100 m sec(exp -1) in a narrow stream, constrained by the addition of an inert gas flow (0.4 torr). The OH molecule is both excited and detected in the A(exp 2)Sigma (v' = 0) yields X(exp 2)II (v'' = 0) transition at 308 nm. Light from a copper vapor-pumped dye laser (rep. rate = 10kHz; pulse length = 20 ns; linewidth = .1 cm(exp -1), and average power = 15 mW), resonant with the Q(sub 1)(3) transition, is multipassed through a White cell and intercepts the air stream as 24 non-overlapping 2mm by 5mm beams. A fast microchannel plate detector is turned off during the laser pulse to prevent saturation of the detector due to Rayleigh and chamber scattering. It is turned on 30-100 nsec after the end of the laser pulse for 300 ns to collect resonance fluorescence from OH. HO2 is detected by chemical conversion to OH by reaction with reagent NO, followed by OH detection. Both the detection sensitivity and the inlet characteristics must be understood for any in situ instrument. For the calibration of the detection sensitivity, OH is produced quantitatively by the fast H + NO2 yields OH + NO reaction in a low pressure, flowing discharge tube connected to the detection chamber. The inlet transmission of OH inlet is calibrated separately.

Conditioning of the vacuum system of the TPS storage ring without baking in situ

NASA Astrophysics Data System (ADS)

Chan, C. K.; Chang, C. C.; Shueh, C.; Yang, I. C.; Wu, L. H.; Chen, B. Y.; Cheng, C. M.; Huang, Y. T.; Chuang, J. Y.; Cheng, Y. T.; Hsiao, Y. M.; Sheng, Albert

2017-04-01

To shorten the machine downtime, a maintenance procedure without baking in situ has been developed and applied to maintain and to upgrade the vacuum system of the TPS storage ring. The data of photon-stimulated desorption (PSD) reveal no obvious discrepancy between baking and not baking the vacuum system in situ. A beam-conditioning dose of extent only 11.8 A h is required to recover quickly the dynamic pressure of an unbaked vacuum system to its pre-intervention value according to the TPS maintenance experience.

In Situ Visualization of the Dynamics in Xylem Embolism Formation and Removal in the Absence of Root Pressure: A Study on Excised Grapevine Stems.

PubMed

Knipfer, Thorsten; Cuneo, Italo F; Brodersen, Craig R; McElrone, Andrew J

2016-06-01

Gas embolisms formed during drought can disrupt long-distance water transport through plant xylem vessels, but some species have the ability to remove these blockages. Despite evidence suggesting that embolism removal is linked to the presence of vessel-associated parenchyma, the underlying mechanism remains controversial and is thought to involve positive pressure generated by roots. Here, we used in situ x-ray microtomography on excised grapevine stems to determine if embolism removal is possible without root pressure, and if the embolism formation/removal affects vessel functional status after sample excision. Our data show that embolism removal in excised stems was driven by water droplet growth and was qualitatively identical to refilling in intact plants. When stem segments were rehydrated with H2O after excision, vessel refilling occurred rapidly (<1 h). The refilling process was substantially slower when polyethylene glycol was added to the H2O source, thereby providing new support for an osmotically driven refilling mechanism. In contrast, segments not supplied with H2O showed no refilling and increased embolism formation. Dynamic changes in liquid/wall contact angles indicated that the processes of embolism removal (i.e. vessel refilling) by water influx and embolism formation by water efflux were directly linked to the activity of vessel-associated living tissue. Overall, our results emphasize that root pressure is not required as a driving force for vessel refilling, and care should be taken when performing hydraulics measurements on excised plant organs containing living vessel-associated tissue, because the vessel behavior may not be static. © 2016 American Society of Plant Biologists. All Rights Reserved.

Rapid in situ assessment of physiological activities in bacterial biofilms using fluorescent probes

NASA Technical Reports Server (NTRS)

Yu, F. P.; McFeters, G. A.

1994-01-01

Two rapid in situ enumeration methods using fluorescent probes were used to assess the physiological activities of Klebsiella pneumoniae biofilms on stainless steel. Fluorescent dyes, 5-cyano-2,3-ditolyl tetrazolium chloride (CTC) and rhodamine 123 (Rh 123), were chosen to perform this study. CTC is a soluble redox indicator which can be reduced by respiring bacteria to fluorescent CTC-formazan crystals. Rh 123 is incorporated into bacteria with respect to cellular proton motive force. The intracellular accumulation of these fluorescent dyes can be determined using epifluorescence microscopy. The results obtained with these two fluorescent probes in situ were compared to the plate count (PC) and in situ direct viable count (DVC) methods. Viable cell densities within biofilms determined by the three in situ methods were comparable and always showed approximately 2-fold higher values than those obtained with the PC method. As an additional advantage, the results were observed after 2 h, which was shorter than the 4 h incubation time required for the DVC method and 24 h for colony formation. The results indicate that staining with CTC and Rh 123 provides rapid information regarding cell numbers and physiological activities of bacteria within biofilms.

Wind Tunnel Application of a Pressure-Sensitive Paint Technique to a Faceted Missile Model at Subsonic and Transonic Speeds

NASA Technical Reports Server (NTRS)

Erickson, Gary E.

2004-01-01

A pressure-sensitive paint (PSP) technique was applied in a wind tunnel experiment in the NASA Langley Research Center 8-Foot Transonic Pressure Tunnel to quantify the vortex-induced surface static pressures on a slender, faceted missile model at subsonic and transonic speeds. Satisfactory global calibrations of the PSP were obtained at =0.70, 0.90, and 1.20, angles of attack from 10 degrees to 20 degrees, and angles of sideslip of 0 and 2.5 degrees using an in-situ method featuring the simultaneous acquisition of electronically-scanned pressures (ESP) at 57 discrete locations on the model. Both techniques clearly revealed the significant influence on the surface pressure distributions of the vortices shed from the sharp, chine-like leading edges. The mean error in the PSP measurements relative to the ESP data was approximately 0.6 percent at M infinity =0.70 and 2.6 percent at M infinity =0.90 and 1.20. The vortex surface pressure signatures obtained from the PSP and ESP techniques were correlated with the off-surface vortex cross-flow structures obtained using a laser vapor screen (LVS) flow visualization technique. The on-surface and off-surface techniques were complementary, since each provided details of the vortex-dominated flow that were not clear or apparent in the other.

Sub-Kelvin magnetic and electrical measurements in a diamond anvil cell with in-situ tunability

DOE PAGES

Palmer, Alexander; Silevitch, Daniel; Feng, Yejun; ...

2015-09-04

We discuss techniques for performing continuous measurements across a wide range of pressure-field-temperature phase space, combining the milli-Kelvin temperatures of a helium dilution refrigerator with that of the giga-Pascal pressures of a diamond anvil cell and the Tesla magnetic fields of a superconducting magnet. With a view towards minimizing remnant magnetic fields and background magnetic susceptibility, we then characterize high-strength superalloy materials for the pressure cell assembly, which allows high fidelity measurements of low-field phenomena such as superconductivity below 100 mK at pressures above 10 GPa. In situ tunability and measurement of the pressure permit experiments over a wide rangemore » of pressure, while at the same time making possible precise steps across abrupt phase transitions such as that from insulator to metal.« less

Constraints on Pore Pressure in Subduction Zones From Geotechnical Tests and Physical Properties Data

NASA Astrophysics Data System (ADS)

Saffer, D. M.; McKiernan, A. W.

2005-12-01

At subduction zones, as incoming sediments are either offscraped or underthrust at the trench, elevated pore pressures result from the combination of rapid loading and low permeability. Pore pressure within underthrust sediment is especially important for the mechanical strength of the plate boundary fault system, because the main décollement localizes immediately above this sediment, and at many subduction zones steps downward into it. Because the underthrust sediment undergoes progressive uniaxial (vertical) strain, quantitative estimates of in situ pore pressure can be obtained by several methods, including: (1) maximum past burial stress ( Pv'}) from laboratory consolidation tests on core samples, and (2) observed compaction trends in boreholes. These methods allow a detailed view of pore pressure and its variability down-section, providing insight into dewatering processes and the evolution of shear strength relevant to early development of the décollement. Geotechnical tests also provide independent measurement of the coefficient of consolidation ( Cv), compressibility ( mv), and permeability (k) of sediment samples, which can be used to parameterize forward models of pressure generation. Here, I discuss pore pressure estimates derived from (1) consolidation tests on core samples, and (2) observed porosity profiles, along transects where ODP drilling has sampled sediment at the Nankai, N. Barbados, and Costa Rican subduction zones. At all three margins, the two independent methods yield consistent results, and indicate development of significant overpressures that increase systematically with distance from the trench. The values are in good agreement with direct measurements in 2 instrumented boreholes at Barbados, maximum and minimum bounds from the known loading rate, and results of 2-D numerical models of fluid flow. Inferred pressures document nearly undrained conditions at the base of the section (excess pressures equal to the load emplaced by

In situ field measurement of leaf water potential using thermocouple psychrometers.

PubMed

Savage, M J; Wiebe, H H; Cass, A

1983-11-01

Thermocouple psychrometers are the only instruments which can measure the in situ water potential of intact leaves, and which can possibly be used to monitor leaf water potential. Unfortunately, their usefulness is limited by a number of difficulties, among them fluctuating temperatures and temperature gradients within the psychrometer, sealing of the psychrometer chamber to the leaf, shading of the leaf by the psychrometer, and resistance to water vapor diffusion by the cuticle when the stomates are closed. Using Citrus jambhiri, we have tested several psychrometer design and operational modifications and showed that in situ psychrometric measurements compared favorably with simultaneous Scholander pressure chamber measurements on neighboring leaves when the latter were corrected for the osmotic potential.

Nitrogen removal from landfill leachate via ex situ nitrification and sequential in situ denitrification

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

Zhong Qi; Graduate School of Chinese Academy of Sciences, Beijing 100049; Li Daping

2009-04-15

Ex situ nitrification and sequential in situ denitrification represents a novel approach to nitrogen management at landfills. Simultaneous ammonia and organics removal was achieved in a continuous stirred tank reactor (CSTR). The results showed that the maximum nitrogen loading rate (NLR) and the maximum organic loading rate (OLR) was 0.65 g N l{sup -1} d{sup -1} and 3.84 g COD l{sup -1} d{sup -1}, respectively. The ammonia and chemical oxygen demand (COD) removal was over 99% and 57%, respectively. In the run of the CSTR, free ammonia (FA) inhibition and low dissolved oxygen (DO) were found to be key factorsmore » affecting nitrite accumulation. In situ denitrification was studied in a municipal solid waste (MSW) column by recalculating nitrified leachate from CSTR. The decomposition of MSW was accelerated by the recirculation of nitrified leachate. Complete reduction of total oxidized nitrogen (TON) was obtained with maximum TON loading of 28.6 g N t{sup -1} TS d{sup -1} and denitrification was the main reaction responsible. Additionally, methanogenesis inhibition was observed while TON loading was over 11.4 g N t{sup -1} TS d{sup -1} and the inhibition was enhanced with the increase of TON loading.« less

Sensor-model prediction, monitoring and in-situ control of liquid RTM advanced fiber architecture composite processing

NASA Technical Reports Server (NTRS)

Kranbuehl, D.; Kingsley, P.; Hart, S.; Loos, A.; Hasko, G.; Dexter, B.

1992-01-01

In-situ frequency dependent electromagnetic sensors (FDEMS) and the Loos resin transfer model have been used to select and control the processing properties of an epoxy resin during liquid pressure RTM impregnation and cure. Once correlated with viscosity and degree of cure the FDEMS sensor monitors and the RTM processing model predicts the reaction advancement of the resin, viscosity and the impregnation of the fabric. This provides a direct means for predicting, monitoring, and controlling the liquid RTM process in-situ in the mold throughout the fabrication process and the effects of time, temperature, vacuum and pressure. Most importantly, the FDEMS-sensor model system has been developed to make intelligent decisions, thereby automating the liquid RTM process and removing the need for operator direction.

Atmospheric Balloon Swarms for Persistent In-Situ Measurements in Hurricanes

NASA Astrophysics Data System (ADS)

Meneghello, G.; Bewley, T.

2015-12-01

Real-time measurements within hurricanes are essential to improve forecasts, protect property and save lives. Current methods for obtaining in-situ data, including radar and satellite imagery as well as drop-sondes deployed from repeated aircraft flights above or even within the hurricane itself, are costly, dangerous and limited in duration or resolution. We demonstrate how a swarm of inexpensive, buoyancy-controlled, sensor-laden balloons can be deployed from altitude or from sea-level within a hurricane flow field, and coordinated autonomously in an energetically-efficient fashion to persistently and continuously monitor relevant properties (pressure, humidity, temperature, windspeed) of a hurricane for days at a time. Rather than fighting the gale-force winds in the storm, the strong, predictable stratification of these winds is leveraged to disperse the balloons into a favorable, time-evolving distribution and to follow the hurricane track as it moves. Certain target orbits of interest in the hurricane can be continuously sampled by some balloons, while other balloons make continuous sweeps between the eye and the spiral rain bands. We expect the acquired data to complement current measurement methods and to be instrumental in improving the numerical models' forecast skills.

In situ electronic probing of semiconducting nanowires in an electron microscope.

PubMed

Fauske, V T; Erlbeck, M B; Huh, J; Kim, D C; Munshi, A M; Dheeraj, D L; Weman, H; Fimland, B O; Van Helvoort, A T J

2016-05-01

For the development of electronic nanoscale structures, feedback on its electronic properties is crucial, but challenging. Here, we present a comparison of various in situ methods for electronically probing single, p-doped GaAs nanowires inside a scanning electron microscope. The methods used include (i) directly probing individual as-grown nanowires with a sharp nano-manipulator, (ii) contacting dispersed nanowires with two metal contacts and (iii) contacting dispersed nanowires with four metal contacts. For the last two cases, we compare the results obtained using conventional ex situ litho-graphy contacting techniques and by in situ, direct-write electron beam induced deposition of a metal (Pt). The comparison shows that 2-probe measurements gives consistent results also with contacts made by electron beam induced deposition, but that for 4-probe, stray deposition can be a problem for shorter nanowires. This comparative study demonstrates that the preferred in situ method depends on the required throughput and reliability. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

In Situ Deformation of Olivine in the Transmission Electron Microscope: from Dislocation Velocity Measurements to Stress-Strain Curves

NASA Astrophysics Data System (ADS)

Bollinger, C.; Idrissi, H.; Boioli, F.; Cordier, P.

2015-12-01

There is a growing consensus to recognize that rheological law established for olivine at high-temperature (ca. >1000°C) fail when extrapolated to low temperatures relevant for the lithospheric mantle. Hence it appears necessary to fit rheological laws against data at low temperatures where olivine tends to become more and more brittle. The usual approach consists in applying confining pressure to inhibit brittleness. Here we propose an innovative approach based on the use of very small samples and numerical modelling. New commercial in situ TEM nanotensile testing equipment recently developed by Hysitron.Inc is combined with weak-beam dark-field TEM diffraction contrast imaging in order to obtain information on the elementary mechanisms controlling the plasticity of olivine: namely glide of [001] screw dislocations. The olivine tensile beams dedicated for in situ TEM nanomechanical testing were produced using microfabrication techniques based on MEMS-type procedures. The testing geometry was designed as to induce maximum resolved shear stresses on the [001](110) slip system. Under tensile loads between 2 and 3 GPa, ductile behaviour was reached with the development and propagation of dislocation loops across the sample allowing to measure the velocity of screw and non-screw dislocations as a function of stress. This information is introduced into a numerical model involving Dislocation Dynamics in order to obtain the stress-strain curves describing the mechanical response of olivine single crystals deformed in tension at room temperature.

Exploration of CdTe quantum dots as mesoscale pressure sensors via time-resolved shock-compression photoluminescent emission spectroscopy

NASA Astrophysics Data System (ADS)

Kang, Zhitao; Banishev, Alexandr A.; Lee, Gyuhyon; Scripka, David A.; Breidenich, Jennifer; Xiao, Pan; Christensen, James; Zhou, Min; Summers, Christopher J.; Dlott, Dana D.; Thadhani, Naresh N.

2016-07-01

The nanometer size of CdTe quantum dots (QDs) and their unique optical properties, including size-tunable narrow photoluminescent emission, broad absorption, fast photoluminescence decay, and negligible light scattering, are ideal features for spectrally tagging the shock response of localized regions in highly heterogeneous materials such as particulate media. In this work, the time-resolved laser-excited photoluminescence response of QDs to shock-compression was investigated to explore their utilization as mesoscale sensors for pressure measurements and in situ diagnostics during shock loading experiments. Laser-driven shock-compression experiments with steady-state shock pressures ranging from 2.0 to 13 GPa were performed on nanocomposite films of CdTe QDs dispersed in a soft polyvinyl alcohol polymer matrix and in a hard inorganic sodium silicate glass matrix. Time-resolved photoluminescent emission spectroscopy was used to correlate photoluminescence changes with the history of shock pressure and the dynamics of the matrix material surrounding the QDs. The results revealed pressure-induced blueshifts in emitted wavelength, decreases in photoluminescent emission intensity, reductions in peak width, and matrix-dependent response times. Data obtained for these QD response characteristics serve as indicators for their use as possible time-resolved diagnostics of the dynamic shock-compression response of matrix materials in which such QDs are embedded as in situ sensors.

In situ metrology to characterize water vapor delivery during atomic layer deposition

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

Ahmido, Tariq, E-mail: tariq.ahmido@nist.gov; Kimes, William A.; Sperling, Brent A.

Water is often employed as the oxygen source in metal oxide atomic layer deposition (ALD) processes. It has been reported that variations in the amount of water delivered during metal oxide ALD can impact the oxide film properties. Hence, one contribution to optimizing metal oxide ALD processes would be to identify methods to better control water dose. The development of rapid, quantitative techniques for in situ water vapor measurements during ALD processes would be beneficial to achieve this goal. In this report, the performance of an in situ tunable diode laser absorption spectroscopy (TDLAS) scheme for performing rapid, quantitative watermore » partial pressure measurements in a representative quarter-inch ALD delivery line is described. This implementation of TDLAS, which utilizes a near-infrared distributed-feedback diode laser and wavelength modulation spectroscopy, provides measurements of water partial pressure on a timescale comparable to or shorter than the timescale of the gas dynamics in typical ALD systems. Depending on the degree of signal averaging, this TDLAS system was capable of measuring the water partial pressure with a detection limit in the range of ∼0.80 to ∼0.08 Pa. The utility of this TDLAS scheme was demonstrated by using it to identify characteristics of a representative water delivery system that otherwise would have been difficult to predict. Those characteristics include (1) the magnitude and time dependence of the pressure transient that can occur during water injection, and (2) the dependence of the steady-state water partial pressure on the carrier gas flow rate and the setting of the water ampoule flow restriction.« less

Study on the release of fenofibrate nanosuspension in vitro and its correlation with in situ intestinal and in vivo absorption kinetics in rats.

PubMed

Xu, Yuanlong; Wang, Yonglu; Li, Xue Ming; Huang, Qinqin; Chen, Wei; Liu, Ran; Chen, BaoAn; Wei, Ping

2014-07-01

As an oral delivery carrier for poorly water soluble drugs, the nanosuspension was prepared by melt emulsification method combined with high-pressure homogenization. The objective of this study was to clarify the absorption mechanism in rats of fenofibrate nanosuspension using the model of in situ gut perfusion. The release rate of drug from nanosuspension was fast which about 70% of the drug would be released within 5 minutes. The absorption of fenofibrate nanosuspension in the gastrointestinal (GI) tract was studied by the in situ closed loop method in rats. It was found that the absorption process in intestine was first-process with passive diffusion mechanism, and the whole intestine was the major segment for the drug absorption. Additionally, GI absorption in situ studies indicated that the fenofibrate nanosuspension had great success in regard to enhancement of intestinal absorption compared to the fenofibrate suspension of coarse powder. The pharmacokinetic characteristics were studied in rats after oral administration of fenofibrate nanosuspension or suspension at the dosage of 27 mg/kg. The plasma concentration-time curve was fitted to the one-compartment model. The correlation between in vitro dissolution (P), in situ intestinal absorption (F) and in vivo absorption (Fa) in rats was investigated with the results as follows: Fa = 6.2061P-456.38(r = 0.9559), F = 3.6911P-2.2169(r = 0.970), F = 0.5095P + 44.189(r = 0.9609). The highest level A could be obtained from the in vitro--in vivo correlation (IVIVC) between dissolution percentage and intestinal absorption of the fenofibrate nanosuspension in rats. Consequently, the in situ intestinal perfusion model could be used to predict the in vivo pharmacokinetic characteristics in rats.

Pressure-Sensitive Paint Investigation of Double-Delta Wing Vortex Flow Manipulation

NASA Technical Reports Server (NTRS)

Erickson, Gary E.; Gonzalez, Hugo A.

2004-01-01

A pressure-sensitive paint (PSP) technique was applied in a wind tunnel experiment in the NASA Langley Research Center 8-Foot Transonic Pressure Tunnel to quantify the effect of wing fillets on the global vortex-induced surface static pressure field about a sharp leading-edge 76o/40o double delta wing, or strake-wing, model at subsonic and transonic speeds. Global calibrations of the PSP were obtained at M = 0.50, 0.70, 0.85, 0.95, and 1.20, a Reynolds number per unit length of 2.0 million, and angles of attack from 10 degrees to 20 degrees using an in-situ method featuring the simultaneous acquisition of electronically-scanned pressures (ESP) at discrete locations on the model. The mean error in the PSP measurements relative to the ESP data was approximately 2 percent or less at M = 0.50 to 0.85 but increased to several percent at M =0.95 and 1.20. The PSP pressure distributions and pseudo-colored planform view pressure maps clearly revealed the vortex-induced pressure signatures at all Mach numbers and angles of attack. Small fillets having a parabolic or diamond planform situated at the strake-wing intersection were designed to manipulate the vortical flows by, respectively, removing the leading-edge discontinuity or introducing additional discontinuities. The fillets caused global changes in the vortex-dominated surface pressure field that were effectively captured in the PSP measurements. The vortex surface pressure signatures were compared to available off-surface vortex cross-flow structures obtained using a laser vapor screen (LVS) flow visualization technique. The fillet effects on the PSP pressure distributions and the observed leading-edge vortex flow characteristics were consistent with the trends in the measured lift, drag, and pitching moment coefficients.

Pressure-Sensitive Paint Investigation of Double-Delta Wing Vortex Flow Manipulation

NASA Technical Reports Server (NTRS)

Erickson, Gary E.; Gonzalez, Hugo A.

2005-01-01

A pressure-sensitive paint (PSP) technique was applied in a wind tunnel experiment in the NASA Langley Research Center 8-Foot Transonic Pressure Tunnel to quantify the effect of wing fillets on the global vortex-induced surface static pressure field about a sharp leading-edge 76 deg/40 deg double delta wing, or strake-wing, model at subsonic and transonic speeds. Global calibrations of the PSP were obtained at M = 0.50, 0.70, 0.85, 0.95, and 1.20, a Reynolds number per unit length of 2.0 million, and angles of attack from 10 degrees to 30 degrees using an in-situ method featuring the simultaneous acquisition of electronically-scanned pressures (ESP) at discrete locations on the model. The mean error in the PSP measurements relative to the ESP data was approximately 2 percent or less at M = 0.50 to 0.85 but increased to several percent at M = 0.95 and 1.20. The PSP pressure distributions and pseudo-colored planform view pressure maps clearly revealed the vortex-induced pressure signatures at all Mach numbers and angles of attack. Small fillets having a parabolic or diamond planform situated at the strake-wing intersection were designed to manipulate the vortical flows by, respectively, removing the leading-edge discontinuity or introducing additional discontinuities. The fillets caused global changes in the vortex-dominated surface pressure field that were effectively captured in the PSP measurements. The vortex surface pressure signatures were compared to available off-surface vortex cross-flow structures obtained using a laser vapor screen (LVS) flow visualization technique. The fillet effects on the PSP pressure distributions and the observed leading-edge vortex flow characteristics were consistent with the trends in the measured lift, drag, and pitching moment coefficients.

In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

NASA Astrophysics Data System (ADS)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Zhao, Tiejun; Esmaeili, Morteza; Diaz, Ana; Andreasen, Jens W.; Mathiesen, Ragnvald H.; Rønning, Magnus; Breiby, Dag W.

2014-06-01

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Powdered Magnesium-Carbon Dioxide Rocket Combustion Technology for In Situ Mars Propulsion

NASA Technical Reports Server (NTRS)

Foote, J. P.; Litchford, R. J.

2007-01-01

Powdered magnesium (Mg) carbon dioxide (CO2) combustion is examined as a potential in situ propellant combination for Mars propulsion. Although this particular combination has relatively low performance in comparison to traditional bipropellants, it remains attractive as a potential basis for future martian mobility systems, since it could be partially or wholly manufactured from indigenous planetary resources. As a means of achieving high mobility during long-duration Mars exploration missions, the poorer performing in situ combination can, in fact, become a superior alternative to conventional storable propellants, which would need to be entirely transported from Earth. Thus, the engineering aspects of powdered metal combustion devices are discussed including transport/injection of compacted powder, ignition, combustion efficiency, combustion stability, dilution effects, lean burn limits, and slag formation issues. It is suggested that these technological issues could be effectively addressed through a multiphase research and development effort beginning with basic feasibility tests using an existing dump configured atmospheric pressure burner. Follow-on phases would involve the development and testing of a pressurized research combustor and technology demonstration tests of a prototypical rocket configuration.

All-fiber optoelectronic sensor with Bragg gratings for in-situ cure monitoring

NASA Astrophysics Data System (ADS)

Cusano, Andrea; Breglio, Giovanni; Cutolo, Antonello; Calabro, Antonio M.; Giordano, Michele; Nicolais, Luigi, II

2000-08-01

Real-time, in situ monitoring for quality control of the polymer cure process is of high interest, since thermoset polymer-matrix composite are widely used in large industrial areas: aeronautical, aerospace, automotive and civil due to their low cost/low weight features. However, their final properties are strongly dependence on the processing parameters, such as temperature and pressure sequence. The key-point for advanced composite materials is the possibility to have distributed and simultaneous monitoring of chemoreological and physical properties during the cure process. To this aim, we have developed and tested an optoelectronic fiber optic sensor based on the Fresnel principle able to monitor the variations of the refractive index due to the cure process of an epoxy based resin. Experimental results have been obtained on sensor capability to monitor the cure kinetics by assuming the refractive index as reaction co-ordinate. The integration with in-fiber Bragg grating in order to measure the local temperature has been discussed and tested.

HYDRAULIC FRACTURING IN PORUS AND NONPORUS ROCK AND ITS POTENTIAL FOR DETERMINING IN-SITU STRESSES AT GREAT DEPTH.

DTIC Science & Technology

The process of Hydraulic Fracturing as a method of determining in-situ stresses in brittle elastic formations at great depth is analyzed both...theoretically and experimentally. Theoretically, it is found that in attempting to relate the recorded hydraulic fracturing pressures to tectonic stresses...at great depth. The experimental results show that hydraulic fracturing occurred when the internal pressure achieved a critical value that could

In-Situ Nondestructive Evaluation of Kevlar(Registered Trademark)and Carbon Fiber Reinforced Composite Micromechanics for Improved Composite Overwrapped Pressure Vessel Health Monitoring

NASA Technical Reports Server (NTRS)

Waller, Jess; Saulsberry, Regor

2012-01-01

NASA has been faced with recertification and life extension issues for epoxy-impregnated Kevlar 49 (K/Ep) and carbon (C/Ep) composite overwrapped pressure vessels (COPVs) used in various systems on the Space Shuttle and International Space Station, respectively. Each COPV has varying criticality, damage and repair histories, time at pressure, and pressure cycles. COPVs are of particular concern due to the insidious and catastrophic burst-before-leak failure mode caused by stress rupture (SR) of the composite overwrap. SR life has been defined [1] as the minimum time during which the composite maintains structural integrity considering the combined effects of stress level(s), time at stress level(s), and associated environment. SR has none of the features of predictability associated with metal pressure vessels, such as crack geometry, growth rate and size, or other features that lend themselves to nondestructive evaluation (NDE). In essence, the variability or surprise factor associated with SR cannot be eliminated. C/Ep COPVs are also susceptible to impact damage that can lead to reduced burst pressure even when the amount of damage to the COPV is below the visual detection threshold [2], thus necessitating implementation of a mechanical damage control plan [1]. Last, COPVs can also fail prematurely due to material or design noncompliance. In each case (SR, impact or noncompliance), out-of-family behavior is expected leading to a higher probability of failure at a given stress, hence, greater uncertainty in performance. For these reasons, NASA has been actively engaged in research to develop NDE methods that can be used during post-manufacture qualification, in-service inspection, and in-situ structural health monitoring. Acoustic emission (AE) is one of the more promising NDE techniques for detecting and monitoring, in real-time, the strain energy release and corresponding stress-wave propagation produced by actively growing flaws and defects in composite

Monitoring nanoparticle synthesis in a carbon arc discharge environment, in situ

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

Mitrani, James

This work presents experimental and theoretical studies of gas-phase synthesis of fullerenes and carbon nanoparticles in the presence of an atmospheric-pressure, arc discharge plasma. Carbon arc discharges have been used for synthesizing carbon nanotubes for over 25 years, and have the potential for economically synthesizing industrial-scale quantities of fullerenes. However, the efficiency and selectivity of fullerene synthesis with carbon arc discharges are quite low. Optimizing carbon arc discharges for fullerene synthesis requires a thorough understanding of the dynamics behind gas-phase nanoparticle synthesis in the presence of an arc discharge plasma. We built a carbon arc discharge setup to study nanoparticlemore » and fullerene synthesis. The laser-induced incandescence (LII) diagnostic was applied for monitoring nanoparticle synthesis, in situ. The LII diagnostic had previously been applied as a combustion diagnostic for in situ measurements of concentrations and sizes of soot particles in flame environments. Prior to the present study, it had never been applied for studying fullerenes, nor had it been applied to study nanoparticles in the presence of an atmospheric-pressure plasma. Therefore, experiments were designed that allowed for the calibration of the LII diagnostic with research-grade, arc-synthesized soot particles and carbon nanotubes. Additionally, the theory and models underpinning the LII diagnostic were adapted to include the presence of an atmospheric-pressure, arc-discharge plasma. Results presented in this work confirm the ability of the LII diagnostic to measure sizes of arc-synthesized nanoparticles in situ, and show the spatial location of high densities of arc-synthesized nanoparticles with respect to the arc discharge plasma. Determining the spatial location of nanoparticle synthesis and growth is crucial for understanding the background conditions (e.g. background gas temperature, electron densities ...) in which nanoparticles

Sub-Kelvin magnetic and electrical measurements in a diamond anvil cell with in situ tunability

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

Palmer, A; Silevitch, D M; Feng, Yejun

2015-09-01

We discuss techniques for performing continuous measurements across a wide range of pressure–field–temperature phase space, combining the milli-Kelvin temperatures of a helium dilution refrigerator with the giga-Pascal pressures of a diamond anvil cell and the Tesla magnetic fields of a superconducting magnet. With a view towards minimizing remnant magnetic fields and background magnetic susceptibility, we characterize high-strength superalloy materials for the pressure cell assembly, which allows high fidelity measurements of low-field phenomena such as superconductivity below 100 mK at pressures above 10 GPa. In situ tunability and measurement of the pressure permit experiments over a wide range of pressure, whilemore » at the same time making possible precise steps across abrupt phase transitions such as those from insulator to metal.« less

In Situ Powder Diffraction Studies of Electrode Materials in Rechargeable Batteries.

PubMed

Sharma, Neeraj; Pang, Wei Kong; Guo, Zaiping; Peterson, Vanessa K

2015-09-07

The ability to directly track the charge carrier in a battery as it inserts/extracts from an electrode during charge/discharge provides unparalleled insight for researchers into the working mechanism of the device. This crystallographic-electrochemical information can be used to design new materials or modify electrochemical conditions to improve battery performance characteristics, such as lifetime. Critical to collecting operando data used to obtain such information in situ while a battery functions are X-ray and neutron diffractometers with sufficient spatial and temporal resolution to capture complex and subtle structural changes. The number of operando battery experiments has dramatically increased in recent years, particularly those involving neutron powder diffraction. Herein, the importance of structure-property relationships to understanding battery function, why in situ experimentation is critical to this, and the types of experiments and electrochemical cells required to obtain such information are described. For each battery type, selected research that showcases the power of in situ and operando diffraction experiments to understand battery function is highlighted and future opportunities for such experiments are discussed. The intention is to encourage researchers to use in situ and operando techniques and to provide a concise overview of this area of research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In situ detrital zircon (U-Th)/He thermochronology

NASA Astrophysics Data System (ADS)

Tripathy, A.; Monteleone, B. D.; van Soest, M. C.; Hodges, K.; Hourigan, J. K.

2010-12-01

Detrital studies of both sand and rock are relevant to many problems, ranging from the climate and tectonics feedback debate to the long-term record of orogenic evolution. When applying the conventional (U-Th)/He technique to such studies, two important issues arise. Often, only euhedral grains are permissible for analysis in order to make simple geometric corrections for α-recoil. In detrital samples, this is problematic because euhedral grains can be scarce due to mechanical abrasion during transport, and potentially introduce bias in favour of more proximally sourced grains. Second, inherent to detrital studies is the need to date many grains (>100) per sample to ensure a representative sampling of the sediment source region, thus making robust conventional detrital studies both expensive and time-consuming. UV laser microprobes can improve this by permitting careful targeting of the grain interior away from the α-ejection zone, rendering the α-recoil correction unnecessary, thus eliminating bias toward euhedral grains. In the Noble Gas, Geochemistry, and Geochronology Laboratory at ASU, apatite and zircon have been successfully dated using in situ methods. For this study, the conventional and in situ techniques are compared by dating zircons from a modern river sand that drains a small catchment in the Mesozoic-Cenozoic Ladakh Batholith in NW India. This sample has a simple provenance, which allows us to demonstrate the robustness of the in situ method. Moreover, different microbeam techniques will be explored to establish the most efficient approach to obtain accurate and precise U-Th concentrations using synrock, which is our powdered, homogenized, and reconstituted zircon-rock standard. Without this, such in situ U-Th data would be difficult to obtain. 117 zircons were dated using the conventional (U-Th)/He method, revealing dates ranging from 9.70±0.35 to 106.6±3.5 Ma (2σ) with the major mode at 26 Ma. For comparison, 44 grains were dated using the in

In Situ Visualization of the Dynamics in Xylem Embolism Formation and Removal in the Absence of Root Pressure: A Study on Excised Grapevine Stems1[OPEN

PubMed Central

Knipfer, Thorsten; Cuneo, Italo F.; Brodersen, Craig R.; McElrone, Andrew J.

2016-01-01

Gas embolisms formed during drought can disrupt long-distance water transport through plant xylem vessels, but some species have the ability to remove these blockages. Despite evidence suggesting that embolism removal is linked to the presence of vessel-associated parenchyma, the underlying mechanism remains controversial and is thought to involve positive pressure generated by roots. Here, we used in situ x-ray microtomography on excised grapevine stems to determine if embolism removal is possible without root pressure, and if the embolism formation/removal affects vessel functional status after sample excision. Our data show that embolism removal in excised stems was driven by water droplet growth and was qualitatively identical to refilling in intact plants. When stem segments were rehydrated with H2O after excision, vessel refilling occurred rapidly (<1 h). The refilling process was substantially slower when polyethylene glycol was added to the H2O source, thereby providing new support for an osmotically driven refilling mechanism. In contrast, segments not supplied with H2O showed no refilling and increased embolism formation. Dynamic changes in liquid/wall contact angles indicated that the processes of embolism removal (i.e. vessel refilling) by water influx and embolism formation by water efflux were directly linked to the activity of vessel-associated living tissue. Overall, our results emphasize that root pressure is not required as a driving force for vessel refilling, and care should be taken when performing hydraulics measurements on excised plant organs containing living vessel-associated tissue, because the vessel behavior may not be static. PMID:27208267

In Situ Stem Psychrometry: toward a Physiologically-Based Drought Monitoring Network

NASA Astrophysics Data System (ADS)

KOCH, G. W.; Williams, C.; Ambrose, A.

2012-12-01

Plant water potential is a synoptic variable that integrates soil and atmospheric moisture stress and interacts with plant-internal factors to regulate gas exchange and determine vulnerability to drought-induced hydraulic dysfunction. Despite its importance, methods for measuring water potential are labor intensive. This limitation reduces measurement frequency, likely causes important transient events to be overlooked, and restricts development of a richer understanding of the impacts of integrated water stress on plant and ecosystem function. Recent technological advances have enabled in-situ, automated measurement of branch water potential over periods of weeks to months using stem psychrometers. We evaluated this technology through laboratory and field comparisons to standard pressure chamber measurements and with field installations in temperate forest, semi-arid woodland, and chaparral ecosystems. Performance was highly sensitive to installation procedures. With proper sealing, insulation, and radiation shielding, psychrometers typically differed from pressure chamber measurements by less than 0.2 MPa down to water potentials as low as -7 MPa. Measurements in tall trees reaffirmed the influence of gravity on water potential as previously documented with the pressure chamber. Psychrometer performance in situ was stable for periods of several weeks to months, with tissue wound response degrading sensor operation over time. We conclude that stem psychrometer technology is now suitable to serve as the foundation for a physiologically-based drought monitoring network that can anticipate important ecosystem impacts including changes in whole-system fluxes and mortality events.

Lunar In Situ Materials-Based Habitat Technology Development Efforts at NASA/MSFC

NASA Technical Reports Server (NTRS)

Bodiford, Melanie P.; Burks, K. H.; Perry M. R.; Cooper, R. W.; Fiske, M. R.

2006-01-01

For long duration missions on other planetary bodies, the use of in situ materials will become increasingly critical. As man's presence on these bodies expands, so must the structures to accommodate them including habitats, laboratories, berms, garages, solar storm shelters, greenhouses, etc. The use of in situ materials will significantly offset required launch upmass and volume issues. Under the auspices of the In Situ Fabrication & Repair (ISFR) Program at NASA/Marshall Space Flight Center (MSFC), the Habitat Structures project has been developing materials and construction technologies to support development of these in situ structures. This paper will report on the development of several of these technologies at MSFC's Prototype Development Laboratory (PDL). These technologies include, but are not limited to, development of extruded concrete and inflatable concrete dome technologies based on waterless and water-based concretes, development of regolith-based blocks with potential radiation shielding binders including polyurethane and polyethylene, pressure regulation systems for inflatable structures, production of glass fibers and rebar derived from molten lunar regolith simulant, development of regolithbag structures, and others, including automation design issues. Results to date and planned efforts for FY06 will also be presented.

Successive disorder to disorder phase transitions in ionic liquid [HMIM][BF4] under high pressure

NASA Astrophysics Data System (ADS)

Zhu, Xiang; Yuan, Chaosheng; Li, Haining; Zhu, Pinwen; Su, Lei; Yang, Kun; Wu, Jie; Yang, Guoqiang; Liu, Jing

2016-02-01

In situ high-pressure Raman spectroscopy and synchrotron X-ray diffraction have been employed to investigate the phase behavior of ionic liquid, 1-hexyl-3-methylimidazolium tetrafluoroborate ([HMIM][BF4]) under high pressure up to 20 GPa at room temperature. With increasing pressure, some characteristic bands of [HMIM][BF4] disappear, and some characteristic bands of [HMIM][BF4] display non-monotonic pressure-induced frequency shift and non-monotonic variation of full width at half-maximum. Two successive phase transitions at ˜1.7 GPa and 7.3 GPa have been corroborated by the results above. The glass transition pressure (Pg) of [HMIM][BF4] at ˜7.3 GPa has been obtained by ruby R1 line broadening measurements and analysis of synchrotron X-ray diffraction patterns, and its glass transition mechanism is also analyzed in detail. These facts are suggestive of two successive disorder to disorder phase transitions induced by compression, that is, [HMIM][BF4] serves as a superpressurized glass under the pressure above 7.3 GPa, which is similar to the glassy state at low temperature, and a compression-induced liquid to liquid phase transition in [HMIM][BF4] occurs at ˜1.7 GPa. Besides, the conformational equilibrium of the GAAA conformer and AAAA conformer was converted easily in liquid [HMIM][BF4], while it was difficult to be influenced in glassy state.

In situ speciation of uranium in treated acid mine drainage using the diffusion gradients in thin films technique (DGT).

PubMed

Pedrobom, Jorge Henrique; Eismann, Carlos Eduardo; Menegário, Amauri A; Galhardi, Juliana Aparecida; Luko, Karen Silva; Dourado, Thiago de Araujo; Kiang, Chang Hung

2017-02-01

The exchange membranes P81 and DE81 and Chelex-100 resin were used to perform in situ speciation of uranium in treated acid mine drainage at the Osamu Utsumi mining site, Poços de Caldas city, Southeast Brazil. To investigate possible chemical modifications in the samples during analysis, the three ligands were deployed in situ and in a laboratory (in lab). The results obtained in situ were also compared to a speciation performed using Visual MINTEQ software. Chelex-100 retained total labile U for a period of up to 48 h. The labile U fraction determined by Chelex 100 ranged from 107 ± 6% to 147 ± 44% in situ and from 115 ± 22% to 191 ± 5% in lab. DE81 retained anionic U species up to 8 h, with labile fractions ranging from 37 ± 2% to 76 ± 3% in situ and 34 ± 12% to 180 ± 17% in lab. P81 exhibited a lower efficiency in retaining U species, with concentrations ranging from 6± 2% to 19± 2% in situ and 3± 2% to 18± 2% in lab. The speciation obtained from MINTEQ suggests that the major U species were UO 2 OH + , UO 2 (OH) 3- , UO 2 (OH) 2(aq) , Ca 2 UO 2 (CO 3 ) 3(aq) , CaUO 2 (CO 3 ) 3 2- , UO 2 (CO 3 ) 2 2- , and UO 2 (CO 3 ) 3 4- . This result is in accordance with the results obtained in situ. Differences concerning speciation and the total and soluble U concentrations were observed between the deployments performed in situ and in the laboratory, indicating that U speciation must be performed in situ. Copyright © 2016 Elsevier Ltd. All rights reserved.

In situ monitoring of cocrystals in formulation development using low-frequency Raman spectroscopy.

PubMed

Otaki, Takashi; Tanabe, Yuta; Kojima, Takashi; Miura, Masaru; Ikeda, Yukihiro; Koide, Tatsuo; Fukami, Toshiro

2018-05-05

In recent years, to guarantee a quality-by-design approach to the development of pharmaceutical products, it is important to identify properties of raw materials and excipients in order to determine critical process parameters and critical quality attributes. Feedback obtained from real-time analyses using various process analytical technology (PAT) tools has been actively investigated. In this study, in situ monitoring using low-frequency (LF) Raman spectroscopy (10-200 cm -1 ), which may have higher discriminative ability among polymorphs than near-infrared spectroscopy and conventional Raman spectroscopy (200-1800 cm -1 ), was investigated as a possible application to PAT. This is because LF-Raman spectroscopy obtains information about intermolecular and/or lattice vibrations in the solid state. The monitoring results obtained from Furosemide/Nicotinamide cocrystal indicate that LF-Raman spectroscopy is applicable to in situ monitoring of suspension and fluidized bed granulation processes, and is an effective technique as a PAT tool to detect the conversion risk of cocrystals. LF-Raman spectroscopy is also used as a PAT tool to monitor reactions, crystallizations, and manufacturing processes of drug substances and products. In addition, a sequence of conversion behaviors of Furosemide/Nicotinamide cocrystals was determined by performing in situ monitoring for the first time. Copyright © 2018 Elsevier B.V. All rights reserved.

Pressure scanning choices - Rotary vs electronic

NASA Astrophysics Data System (ADS)

Pemberton, Addison

The choices available for present-day pressure scanning applications are described. Typical pressure scanning applications include wind tunnels, flight testing, turbine engine testing, process control, and laboratory/bench testing. The Scanivalve concept is discussed and it is noted that their use eliminates the cost of multiple individual pressure transducers and their signal conditioners as well as associated wiring for each pressure to be measured. However, they are limited to a maximum acquisition speed of 20 ports/sec/scanner. The advantages of electronic pressure scanners include in-situ calibration on demand, fast data acquisition speed, and high reliability. On the other hand, they are three times more expensive than rotary Scanivalves.

High pressure and temperature optical flow cell for near-infra-red spectroscopic analysis of gas mixtures.

PubMed

Norton, C G; Suedmeyer, J; Oderkerk, B; Fieback, T M

2014-05-01

A new optical flow cell with a new optical arrangement adapted for high pressures and temperatures using glass fibres to connect light source, cell, and spectrometer has been developed, as part of a larger project comprising new methods for in situ analysis of bio and hydrogen gas mixtures in high pressure and temperature applications. The analysis is based on measurements of optical, thermo-physical, and electromagnetic properties in gas mixtures with newly developed high pressure property sensors, which are mounted in a new apparatus which can generate gas mixtures with up to six components with an uncertainty of composition of as little as 0.1 mol. %. Measurements of several pure components of natural gases and biogases to a pressure of 20 MPa were performed on two isotherms, and with binary mixtures of the same pure gases at pressures to 17.5 MPa. Thereby a new method of analyzing the obtained spectra based on the partial density of methane was investigated.

In Situ Field Measurement of Leaf Water Potential Using Thermocouple Psychrometers 1

PubMed Central

Savage, Michael J.; Wiebe, Herman H.; Cass, Alfred

1983-01-01

Thermocouple psychrometers are the only instruments which can measure the in situ water potential of intact leaves, and which can possibly be used to monitor leaf water potential. Unfortunately, their usefulness is limited by a number of difficulties, among them fluctuating temperatures and temperature gradients within the psychrometer, sealing of the psychrometer chamber to the leaf, shading of the leaf by the psychrometer, and resistance to water vapor diffusion by the cuticle when the stomates are closed. Using Citrus jambhiri, we have tested several psychrometer design and operational modifications and showed that in situ psychrometric measurements compared favorably with simultaneous Scholander pressure chamber measurements on neighboring leaves when the latter were corrected for the osmotic potential. PMID:16663267

MEASURING VERTICAL PROFILES OF HYDRAULIC CONDUCTIVITY WITH IN SITU DIRECT-PUSH METHODS

EPA Science Inventory

U.S. EPA (Environmental Protection Agency) staff developed a field procedure to measure hydraulic conductivity using a direct-push system to obtain vertical profiles of hydraulic conductivity. Vertical profiles were obtained using an in situ field device-composed of a
Geopr...

Design and deployment of autoclave pressure vessels for the portable deep-sea drill rig MeBo (Meeresboden-Bohrgerät)

NASA Astrophysics Data System (ADS)

Pape, Thomas; Hohnberg, Hans-Jürgen; Wunsch, David; Anders, Erik; Freudenthal, Tim; Huhn, Katrin; Bohrmann, Gerhard

2017-11-01

Pressure barrels for sampling and preservation of submarine sediments under in situ pressure with the robotic sea-floor drill rig MeBo (Meeresboden-Bohrgerät) housed at the MARUM (Bremen, Germany) were developed. Deployments of the so-called MDP (MeBo pressure vessel) during two offshore expeditions off New Zealand and off Spitsbergen, Norway, resulted in the recovery of sediment cores with pressure stages equaling in situ hydrostatic pressure. While initially designed for the quantification of gas and gas-hydrate contents in submarine sediments, the MDP also allows for analysis of the sediments under in situ pressure with methods typically applied by researchers from other scientific fields (geotechnics, sedimentology, microbiology, etc.). Here we report on the design and operational procedure of the MDP and demonstrate full functionality by presenting the first results from pressure-core degassing and molecular gas analysis.

Determination of vapor pressure of low-volatility compounds using a method to obtain saturated vapor with coated capillary columns.

PubMed

Rittfeldt, L

2001-06-01

The vapor pressures of O-ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX), O-isobutyl S-2-diethylaminoethyl methylphosphonothiolate (RVX), and 2,4-dinitrotoluene (2,4-DNT) were determined with the gas saturation method in temperatures ranging from -12 to 103 degrees C. The saturated vapor was generated using a fused-silica column coated with the compound. This column was placed in a gas chromatograph, and the vapor pressure was determined directly from the detector signal or by sampling on Tenax tubes that were subsequently analyzed. From the linear relationships obtained by plotting log P vs 1/T, the enthalpies of vaporization (deltaHvap) and the vapor pressures at selected temperatures were determined. The vapor pressure of VX at 25 degrees C was 0.110 Pa and the deltaHvap 77.9 kJ x mol(-1). The corresponding results for RVX were 0.082 Pa and 76.6 kJ x mol(-1). The vapor pressure of 2,4-DNT at 72 degrees C (melting point) was determined to 6.0 Pa, and the enthalpies of the solid and the liquid state were 94.2 and 75.3 kJ x mol(-1), respectively. Using capillary columns to generate saturated vapors has three major advantages: short equilibrium time, low consumption of sample, and safe handling of toxic compounds.

Assessing Chronology and Mantle Evolution In-Situ with CODEX

NASA Astrophysics Data System (ADS)

Anderson, F. S.; Levine, J.; Whitaker, T.

2017-12-01

Understanding lunar bombardment history is crucial to understanding the dynamic evolution of the Moon. Using an instrument called CODEX (Chemistry, Organics, and Dating Experiment) intended for in-situ dating [1-5], we have obtained Pb-Pb dates for Martian meteorites Zagami and Northwest Africa (NWA) 7034, and lunar meteorites Miller Range 05035, LaPaz Icefield 02205, and NWA 032. In conjunction with our previous Rb-Sr success, these measurments demonstrate the potential for in-situ measurements of the Moon. Some of these Pb dates are consistent with young age estimates, however, many are consistent with previous anomalously old Pb measurements for lunar and SNC meteorites. Proposed explanations for this paradox include terrestrial Pb contamination, that the SNC's are actually ancient and reset in Rb/Sr, that there are multiple isotopic reservoirs sampled by the impact process, or that multiple reservoirs are sampled during the volcanic emplacement. In the future, we plan to use CODEX to test these hypotheses by making measurements on outcrops in-situ on Mars or the Moon, avoiding terrestrial or impact mixing. If in-situ Rb-Sr and Pb-Pb measurements are not concordant, then we are likely constraining the common Pb signature, and hence mantle evolution, of the Moon or Mars. Alternatively, we are likely obtaining a robust age estimate. References: [1] F. S. Anderson et al. LPSC 1246, 2 (2017); [2] F. S. Anderson et al. LPSC 2957, 2 (2017); [3] S. Beck et al., LPSC, 3001, 2 (2017); [4] T. J. Whitaker et al. LPSC 2328, 2 (2017); [5] F. S. Anderson et al. RCMS 29, 191 (2015);

Pressure calibrants in the hydrothermal diamond-anvil cell

USGS Publications Warehouse

Chou, I.-Ming

2007-01-01

Based on the equation of state of water (EOSW), experimental pressure in the hydrothermal diamond-anvil cell (HDAC) using pure water or dilute aqueous solutions as a pressure medium can be accurately determined at each measured temperature. Consequently, meaningful interpretations can be obtained for observations in the HDAC, which has been widely accepted as a versatile, modern apparatus for hydrothermal experiments. However, this is not true when other pressure media were used because there is no reliable way to determine experimental pressure other than the use of in situ pressure sensors. Most of the available pressure sensors are difficult to apply because they either require expensive facilities to perform the measurements or are unable to provide the accuracy needed for the interpretation of hydrothermal experiments. The only exception is to use the interferometric method to detect the ??-?? quartz transition, although such applications are limited to temperatures above 573??C. In this study, three pressure calibrants were calibrated for applications at lower temperatures, and they were based on visual observation of the ferroelastic phase transitions in BaTiO3 (tetragonal/cubic), Pb3(PO4)2 (monoclinic/trigonal), and PbTiO3 (tetragonal/cubic). For the phase transitions in BaTiO3 and Pb3(PO4)2, the temperature at which twinning disappears during heating was taken as the transition temperature (Ttr); the phase transition pressures (Ptr) can be calculated, respectively, from Ptr (MPa; ??3%) = 0.17 - 21.25 [(Ttr) - 115.3], and Ptr (MPa; ??2%) = 1.00 - 10.62 [(Ttr) - 180.2], where Ttr is in ??C. For the phase transition in PbTiO3, the temperature at which the movement of phase front begins (or ends) on heating (or cooling) was taken as the transition temperature (Ttr,h or Ttr,c), and the phase transition pressures on heating (Ptr,h) and cooling (Ptr,c) can be calculated from Ptr,h (MPa; ??4%) = 7021.7 - 14.235 (Ttr,h), and Ptr,c (MPa; ??4%) = 6831.3 - 14.001 (Ttr

High quality x-ray absorption spectroscopy measurements with long energy range at high pressure using diamond anvil cell.

PubMed

Hong, Xinguo; Newville, Matthew; Prakapenka, Vitali B; Rivers, Mark L; Sutton, Stephen R

2009-07-01

We describe an approach for acquiring high quality x-ray absorption fine structure (XAFS) spectroscopy spectra with wide energy range at high pressure using diamond anvil cell (DAC). Overcoming the serious interference of diamond Bragg peaks is essential for combining XAFS and DAC techniques in high pressure research, yet an effective method to obtain accurate XAFS spectrum free from DAC induced glitches has been lacking. It was found that these glitches, whose energy positions are very sensitive to the relative orientation between DAC and incident x-ray beam, can be effectively eliminated using an iterative algorithm based on repeated measurements over a small angular range of DAC orientation, e.g., within +/-3 degrees relative to the x-ray beam direction. Demonstration XAFS spectra are reported for rutile-type GeO2 recorded by traditional ambient pressure and high pressure DAC methods, showing similar quality at 440 eV above the absorption edge. Accurate XAFS spectra of GeO2 glass were obtained at high pressure up to 53 GPa, providing important insight into the structural polymorphism of GeO2 glass at high pressure. This method is expected be applicable for in situ XAFS measurements using a diamond anvil cell up to ultrahigh pressures.

High quality x-ray absorption spectroscopy measurements with long energy range at high pressure using diamond anvil cell

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

Hong, X.; Newville, M.; Prakapenka, V.B.

We describe an approach for acquiring high quality x-ray absorption fine structure (XAFS) spectroscopy spectra with wide energy range at high pressure using diamond anvil cell (DAC). Overcoming the serious interference of diamond Bragg peaks is essential for combining XAFS and DAC techniques in high pressure research, yet an effective method to obtain accurate XAFS spectrum free from DAC induced glitches has been lacking. It was found that these glitches, whose energy positions are very sensitive to the relative orientation between DAC and incident x-ray beam, can be effectively eliminated using an iterative algorithm based on repeated measurements over amore » small angular range of DAC orientation, e.g., within {+-}3{sup o} relative to the x-ray beam direction. Demonstration XAFS spectra are reported for rutile-type GeO{sub 2} recorded by traditional ambient pressure and high pressure DAC methods, showing similar quality at 440 eV above the absorption edge. Accurate XAFS spectra of GeO{sub 2} glass were obtained at high pressure up to 53 GPa, providing important insight into the structural polymorphism of GeO{sub 2} glass at high pressure. This method is expected be applicable for in situ XAFS measurements using a diamond anvil cell up to ultrahigh pressures.« less

In situ measurement of magnesium carbonate formation from CO2 using static high-pressure and -temperature 13C NMR.

PubMed

Surface, J Andrew; Skemer, Philip; Hayes, Sophia E; Conradi, Mark S

2013-01-02

We explore a new in situ NMR spectroscopy method that possesses the ability to monitor the chemical evolution of supercritical CO(2) in relevant conditions for geological CO(2) sequestration. As a model, we use the fast reaction of the mineral brucite, Mg(OH)(2), with supercritical CO(2) (88 bar) in aqueous conditions at 80 °C. The in situ conversion of CO(2) into metastable and stable carbonates is observed throughout the reaction. After more than 58 h of reaction, the sample was depressurized and analyzed using in situ Raman spectroscopy, where the laser was focused on the undisturbed products through the glass reaction tube. Postreaction, ex situ analysis was performed on the extracted and dried products using Raman spectroscopy, powder X-ray diffraction, and magic-angle spinning (1)H-decoupled (13)C NMR. These separate methods of analysis confirmed a spatial dependence of products, possibly caused by a gradient of reactant availability, pH, and/or a reaction mechanism that involves first forming hydroxy-hydrated (basic, hydrated) carbonates that convert to the end-product, anhydrous magnesite. This carbonation reaction illustrates the importance of static (unmixed) reaction systems at sequestration-like conditions.

The use of high pressure CO2 -facilitated pH swings to enhance in situ product recovery of butyric acid in a two-phase partitioning bioreactor.

PubMed

Peterson, Eric C; Daugulis, Andrew J

2014-11-01

Through the use of high partial pressures of CO2 (pCO2 ) to facilitate temporary pH reductions in two-phase partitioning bioreactors (TPPBs), improved pH dependent partitioning of butyric acid was observed which achieved in situ product recovery (ISPR), alleviating end-product inhibition (EPI) during the production of butyric acid by Clostridium tyrobutyricum (ATCC 25755). Through high pressure pCO2 studies, media buffering effects were shown to be substantially overcome at 60 bar pCO2 , resulting in effective extraction of the organic acid by the absorptive polymer Pebax® 2533, yielding a distribution coefficient (D) of 2.4 ± 0.1 after 1 h of contact at this pressure. Importantly, it was also found that C. tyrobutyricum cultures were able to withstand 60 bar pCO2 for 1 h with no decrease in growth ability when returned to atmospheric pressure in batch reactors after several extraction cycles. A fed-batch reactor with cyclic high pCO2 polymer extraction recovered 92 g of butyric acid to produce a total of 213 g compared to 121 g generated in a control reactor. This recovery reduced EPI in the TPPB, resulting in both higher productivity (0.65 vs. 0.33 g L(-1)  h(-1) ) and yield (0.54 vs. 0.40). Fortuitously, it was also found that repeated high pCO2 -facilitated polymer extractions of butyric acid during batch growth of C. tyrobutyricum lessened the need for pH control, and reduced base requirements by approximately 50%. Thus, high pCO2 -mediated absorptive polymer extraction presents a novel method for improving process performance in butyric acid fermentation, and this technique could be applied to the bioproduction of other organic acids as well. © 2014 Wiley Periodicals, Inc.

In-situ determination of residual specific activity in activated concrete walls of a PET-cyclotron room

NASA Astrophysics Data System (ADS)

Matsumura, H.; Toyoda, A.; Masumoto, K.; Yoshida, G.; Yagishita, T.; Nakabayashi, T.; Sasaki, H.; Matsumura, K.; Yamaya, Y.; Miyazaki, Y.

2018-06-01

In the decommissioning work for concrete walls of PET-cyclotron rooms, an in-situ measurement is expected to be useful for obtaining a contour map of the specific activity on the walls without destroying the structure. In this study, specific activities of γ-ray-emitting radionuclides in concrete walls were determined by using an in-situ measurement method employing a portable Ge semiconductor detector, and compared with the specific activity obtained using the sampling measurement method, at the Medical and Pharmacological Research Center Foundation in Hakui, Ishikawa, Japan. Accordingly, the specific activity could be determined by the in-situ determination method. Since there is a clear correlation between the total specific activity of γ-ray-emitting radionuclides and contact dose rate, the specific activity can be determined approximately by contact dose-rate measurement using a NaI scintillation survey meter. The specific activity of each γ-ray-emitting radionuclide can also be estimated from the contact dose rate using a NaI scintillation survey meter. The in-situ measurement method is a powerful tool for the decommissioning of the PET cyclotron room.

Material Total Mass Loss in Vacuum Obtained From Various Outgassing Systems

NASA Technical Reports Server (NTRS)

Scialdone, John; Isaac, Peggy; Clatterbuck, Carroll; Hunkeler, Ronald

2000-01-01

Several instruments including the Cahn Microbalance, the Knudsen Cell, the micro-CVCM, and the vacuum Thermogravimetric Analyzer (TGA) were used in the testing of a graphite/epoxy (GR/EP) composite that is proposed for use as a rigidizing element of an inflatable deployment system. This GR/EP will be cured in situ. The purpose of this testing is to estimate the gaseous production resulting from the curing of the GR/EP composite, to predict the resulting pressure, and to calculate the required venting. Every test was conducted under vacuum at 125 degrees C for 24 hours. Upon comparison of the results, the ASTM E-595 was noted to have given readings that were consistently lower than those obtained using the other instruments, which otherwise provided similar results. The GR/EP was tested using several different geometric arrangements. This paper describes the analysis evaluating the molecular and continuum flow of the outgassing products issuing from the exit port of the ASTM E-595 system. The effective flow conductance provided by the physical dimensions of the vent passage of the ASTM E-595 system and that of the material sample among other factors were investigated to explain the reduced amount of outgassing released during the 24-hour test period.

Determination of Organic Partitioning Coefficients in Water-Supercritical CO 2 Systems by Simultaneous in Situ UV and Near-Infrared Spectroscopies

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

Bryce, David A.; Shao, Hongbo; Cantrell, Kirk J.

2016-06-07

CO2 injected into depleted oil or gas reservoirs for long-term storage has the potential to mobilize organic compounds and distribute them between sediments and reservoir brines. Understanding this process is important when considering health and environmental risks, but little quantitative data currently exists on the partitioning of organics between supercritical CO2 and water. In this work, a high-pressure, in situ measurement capability was developed to assess the distribution of organics between CO2 and water at conditions relevant to deep underground storage of CO2. The apparatus consists of a titanium reactor with quartz windows, near-infrared and UV spectroscopic detectors, and switchingmore » valves that facilitate quantitative injection of organic reagents into the pressurized reactor. To demonstrate the utility of the system, partitioning coefficients were determined for benzene in water/supercritical CO2 over the range 35-65 °C and approximately 25-150 bar. Density changes in the CO2 phase with increasing pressure were shown to have dramatic impacts on benzene's partitioning behavior. Our partitioning coefficients were approximately 5-15 times lower than values previously determined by ex situ techniques that are prone to sampling losses. The in situ methodology reported here could be applied to quantify the distribution behavior of a wide range of organic compounds that may be present in geologic CO2 storage scenarios.« less

Determination of Organic Partitioning Coefficients in Water-Supercritical CO2 Systems by Simultaneous in Situ UV and Near-Infrared Spectroscopies.

PubMed

Bryce, David A; Shao, Hongbo; Cantrell, Kirk J; Thompson, Christopher J

2016-06-07

CO2 injected into depleted oil or gas reservoirs for long-term storage has the potential to mobilize organic compounds and distribute them between sediments and reservoir brines. Understanding this process is important when considering health and environmental risks, but little quantitative data currently exists on the partitioning of organics between supercritical CO2 and water. In this work, a high-pressure, in situ measurement capability was developed to assess the distribution of organics between CO2 and water at conditions relevant to deep underground storage of CO2. The apparatus consists of a titanium reactor with quartz windows, near-infrared and UV spectroscopic detectors, and switching valves that facilitate quantitative injection of organic reagents into the pressurized reactor. To demonstrate the utility of the system, partitioning coefficients were determined for benzene in water/supercritical CO2 over the range 35-65 °C and approximately 25-150 bar. Density changes in the CO2 phase with increasing pressure were shown to have dramatic impacts on benzene's partitioning behavior. Our partitioning coefficients were approximately 5-15 times lower than values previously determined by ex situ techniques that are prone to sampling losses. The in situ methodology reported here could be applied to quantify the distribution behavior of a wide range of organic compounds that may be present in geologic CO2 storage scenarios.

Exploration of CdTe quantum dots as mesoscale pressure sensors via time-resolved shock-compression photoluminescent emission spectroscopy

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

Kang, Zhitao; School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332-0245; Banishev, Alexandr A.

The nanometer size of CdTe quantum dots (QDs) and their unique optical properties, including size-tunable narrow photoluminescent emission, broad absorption, fast photoluminescence decay, and negligible light scattering, are ideal features for spectrally tagging the shock response of localized regions in highly heterogeneous materials such as particulate media. In this work, the time-resolved laser-excited photoluminescence response of QDs to shock-compression was investigated to explore their utilization as mesoscale sensors for pressure measurements and in situ diagnostics during shock loading experiments. Laser-driven shock-compression experiments with steady-state shock pressures ranging from 2.0 to 13 GPa were performed on nanocomposite films of CdTe QDs dispersedmore » in a soft polyvinyl alcohol polymer matrix and in a hard inorganic sodium silicate glass matrix. Time-resolved photoluminescent emission spectroscopy was used to correlate photoluminescence changes with the history of shock pressure and the dynamics of the matrix material surrounding the QDs. The results revealed pressure-induced blueshifts in emitted wavelength, decreases in photoluminescent emission intensity, reductions in peak width, and matrix-dependent response times. Data obtained for these QD response characteristics serve as indicators for their use as possible time-resolved diagnostics of the dynamic shock-compression response of matrix materials in which such QDs are embedded as in situ sensors.« less

Mechanical Anisotropy and Pressure Induced Structural Changes in Piroxicam Crystals Probed by In Situ Indentation and Raman Spectroscopy

NASA Astrophysics Data System (ADS)

Manimunda, Praveena; Hintsala, Eric; Asif, Syed; Mishra, Manish Kumar

2017-01-01

The ability to correlate mechanical and chemical characterization techniques in real time is both lacking and powerful tool for gaining insights into material behavior. This is demonstrated through use of a novel nanoindentation device equipped with Raman spectroscopy to explore the deformation-induced structural changes in piroxicam crystals. Mechanical anisotropy was observed in two major faces ( 0bar{1}1 ) and (011), which are correlated to changes in the interlayer interaction from in situ Raman spectra recorded during indentation. The results of this study demonstrate the considerable potential of an in situ Raman nanoindentation instrument for studying a variety of topics, including stress-induced phase transformation mechanisms, mechanochemistry, and solid state reactivity under mechanical forces that occur in molecular and pharmaceutical solids.

High-pressure-induced structural changes, amorphization and molecule penetration in MFI microporous materials: a review.

PubMed

Vezzalini, Giovanna; Arletti, Rossella; Quartieri, Simona

2014-06-01

This is a comparative study on the high-pressure behavior of microporous materials with an MFI framework type (i.e. natural mutinaite, ZSM-5 and the all-silica phase silicalite-1), based on in-situ experiments in which penetrating and non-penetrating pressure-transmitting media were used. Different pressure-induced phenomena and deformation mechanisms (e.g. pressure-induced over-hydration, pressure-induced amorphization) are discussed. The influence of framework and extra-framework composition and of the presence of silanol defects on the response to the high pressure of MFI-type zeolites is discussed.

Forsterite [Mg 2 SiO 4 )] Carbonation in Wet Supercritical CO 2 : An in Situ High-Pressure X-ray Diffraction Study

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

Todd Schaef, Herbert; McGrail, Bernard P.; Loring, John L.

2013-01-02

Technological advances have been significant in recent years for managing environmentally harmful emissions (mostly CO2) resulting from combustion of fossil fuels. Deep underground geologic formations are emerging as reasonable options for long term storage of CO2 but mechanisms controlling rock and mineral stability in contact with injected supercritical fluids containing water are relatively unknown. In this paper, we discuss mineral transformation reactions occurring with forsterite (Mg2SiO4) exposed to wet supercritical CO2. Forsterite was selected as it is an important olivine group mineral present in igneous and mafic rocks and has been the subject of a large number of aqueous dissolutionmore » studies that can be compared with non-aqueous fluid tests in this study. Transformation reactions were examined by in situ high pressure x-ray diffraction in the presence of supercritical carbon dioxide (scCO2) containing dissolved water at conditions relevant to carbon sequestration. Under modest pressures (90 bar) and temperatures (50°C), scCO2 saturated with water was found to convert >70 wt% forsterite to a hydrated magnesium carbonate, nesquehonite (MgCO3 •3H2O) and magnesite (MgCO3), after 72 hours of reaction. However, comparable tests with scCO2 at only partial water saturation (82%) showed a significantly slower carbonation rate with only ~30-39 wt% conversion to nesquehonite and no evidence of the anhydrous form (MgCO3). Further decreases in water content of the scCO2 continued to reduce the extent of carbonation, until a critical moisture threshold (~30%) was crossed where forsterite no longer reacted in the presence of the wet scCO2 to form crystalline carbonates. Increasing the temperature to 75°C produced anhydrous magnesium carbonate, magnesite (MgCO3), preceded by the intermediate phase, hydromagnesite [Mg(CO3)4(OH)2 •4H2O]. Measurements conducted during in situ IR experiments at 50°C and 30% saturation identified the presence of an amorphous

Functional materials analysis using in situ and in operando X-ray and neutron scattering

PubMed Central

Peterson, Vanessa K.; Papadakis, Christine M.

2015-01-01

In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them. PMID:25866665

Nanoemulsion-based electrolyte triggered in situ gel for ocular delivery of acetazolamide.

PubMed

Morsi, Nadia; Ibrahim, Magdy; Refai, Hanan; El Sorogy, Heba

2017-06-15

In the present work the antiglaucoma drug, acetazolamide, was formulated as an ion induced nanoemulsion-based in situ gel for ocular delivery aiming a sustained drug release and an improved therapeutic efficacy. Different acetazolamide loaded nanoemulsion formulations were prepared using peanut oil, tween 80 and/or cremophor EL as surfactant in addition to transcutol P or propylene glycol as cosurfactant. Based on physicochemical characterization, the nanoemulsion formulation containing mixed surfactants and transcutol P was selected to be incorporated into ion induced in situ gelling systems composed of gellan gum alone and in combination with xanthan gum, HPMC or carbopol. The nanoemulsion based in situ gels showed a significantly sustained drug release in comparison to the nanoemulsion. Gellan/xanthan and gellan/HPMC possessed good stability at all studied temperatures, but gellan/carbopol showed partial drug precipitation upon storage and was therefore excluded from the study. Gellan/xanthan and gellan/HPMC showed higher therapeutic efficacy and more prolonged intraocular pressure lowering effect relative to that of commercial eye drops and oral tablet. Gellan/xanthan showed superiority over gellan/HPMC in all studied parameters and is thus considered as a promising mucoadhesive nanoemulsion-based ion induced in situ gelling formula for topical administration of acetazolamide. Copyright © 2017. Published by Elsevier B.V.

Acoustic velocity in rift basin mudstones: effects of in situ stress and sample lithology, and its relation to formation strength

NASA Astrophysics Data System (ADS)

Zakharova, N. V.; Goldberg, D.

2017-12-01

Acoustic/sonic velocity (Vp) provides one of the best proxies for formation strength, which is essential for geomechanical modeling and formation evaluation. Vp-strength relations need to be built empirically for specific basins and/or rock types. Since velocity is stress- and frequency-dependent, such relations can be very sensitive to experimental conditions; therefore, it is important to quantify their effect on velocity values. In this study, we present confined velocity and strength measurements for over 70 samples from the Newark Rift basin, a candidate site for carbon sequestration, and one of the largest in a series of the Mesozoic rift basins on the eastern North-American coast. Acoustic velocity measurements were obtained for a range of confining pressures from 0 to 6,000 psi, roughly corresponding to in situ confining pressure range. Although, overall, Vp values tend to increase with increasing pressure, the degree of Vp response to stress varies dramatically from sample to sample, and does not appear to correlate directly to lithology or porosity. Select samples exhibit near-zero change in Vp with increasing confining pressure, while others are characterized by up to 15% Vp change with 3,000 psi increase in confining pressure. Compared to sonic logs, the low-stress Vp values usually underestimate sonic velocities, while high-stress values tend to overestimate them. Therefore, a systematic frequency-dependent core-log difference is not observed in these rift basin formations, but accounting for Vp dependence on confining pressure is important. We quantify the Vp-pressure dependence using laboratory acoustic measurements, and develop depth-dependent Vp-strength relation, which could be used with sonic logs for geomechanical analysis in similar Mesozoic rift basin formations.

Use of multiple sensor technologies for quality control of in situ biogeochemical measurements: A SeaCycler case study

NASA Astrophysics Data System (ADS)

Atamanchuk, Dariia; Koelling, Jannes; Lai, Jeremy; Send, Uwe; Wallace, Douglas

2017-04-01

Over the last two decades observing capacity for the global ocean has increased dramatically. Emerging sensor technologies for dissolved gases, nutrients and bio-optical properties in seawater are allowing extension of in situ observations beyond the traditionally measured salinity, temperature and pressure (CTD). However the effort to extend observations using autonomous instruments and platforms carries the risk of losing the level of data quality achievable through conventional water sampling techniques. We will present results from a case study with the SeaCycler profiling winch focusing on quality control of the in-situ measurements. A total of 13 sensors were deployed from May 2016 to early 2017 on SeaCycler's profiling sensor float, including CTD, dissolved oxygen (O2, 3 sensors), carbon dioxide (pCO2, 2 sensors), nutrients, velocity sensors, fluorometer, transmissometer, single channel PAR sensor, and others. We will highlight how multiple measurement technologies (e.g. for O2 and CO2) complement each other and result in a high quality data product. We will also present an initial assessment of the bio-optical data, their implications for seasonal phytoplankton dynamics and comparisons to climatologies and ocean-color data products obtained from the MODIS satellite.

In situ Raman spectroscopic investigation of zirconium-niobium alloy corrosion under hydrothermal conditions

NASA Astrophysics Data System (ADS)

Maslar, J. E.; Hurst, W. S.; Bowers, W. J.; Hendricks, J. H.

2001-10-01

In situ Raman spectroscopy was employed to investigate corrosion of a zirconium-niobium alloy in air-saturated water at a pressure of 15.5 MPa and temperatures ranging from 22 to 407 °C in an optically accessible flow cell. Monoclinic ZrO 2 (m-ZrO 2) was identified under all conditions after the coupon was heated to 255 °C for 19 h. Cubic ZrO 2 (c-ZrO 2) was tentatively identified in situ during heating at temperatures between 306 and 407 °C, but was not observed under any other conditions. Species tentatively identified as α-CrOOH and a Cr VI and/or Cr III/Cr VI compound were observed in situ during heating at temperatures between 255 and 407 °C, but were not observed under any other conditions. The chromium compounds were identified as corrosion products released from the optical cell and/or flow system.