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At least 1,333 records · Page 74

Infrared study on room-temperature atomic layer deposition of HfO{sub 2} using tetrakis(ethylmethylamino)hafnium and remote plasma-excited oxidizing agents

Room-temperature atomic layer deposition (ALD) of HfO{sub 2} was examined using tetrakis (ethylmethylamino)hafnium (TEMAH) and remote plasma-excited water and oxygen. A growth rate of 0.26 nm/cycle at room temperature was achieved, and the TEMAH adsorption and its oxidization on HfO{sub 2} were investigated by multiple internal reflection infrared absorption spectroscopy. It was observed that saturated adsorption of TEMAH occurs at exposures of ∼1 × 10{sup 5} L (1 L = 1 × 10{sup −6} Torr s) at room temperature, and the use of remote plasma-excited water and oxygen vapor is effective in oxidizing the TEMAH molecules on the HfO{sub 2} surface, to produce OH sites. The infrared study suggested that Hf–OH plays a role as an adsorption site for TEMAH. The reaction mechanism of room temperature HfO{sub 2} ALD is discussed in this paper.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

2-Methylpyridinium/pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olates as potent anticonvulsant agents—synthesis and crystal structure

The molecular salt, 2-methylpyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropy-rimidin-4-olate) (I), is prepared from the ethanolic solution of 1-chloro-2,4-dinitrobenzene, pyrimidine-2,4,6-(1H,3H,5H)-trione (barbituric acid) and 2-methylpyridine at room temperature, and the molecular salt, pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olate (II), is prepared from the same reactants, by dissolving them in hot DMSO and ethanol mixture at 70°C. The structures of I and II are characterized by visible, IR, {sup 1}H-NMR, {sup 13}C-NMR and elemental analysis and confirmed by single crystal X-ray analysis. Both the salts crystallize in triclinic crystal system with sp. gr. <##> } P } 1 }&#x00AF;<!-- ?? --> $ P/bar 1 $ P 1-bar </##>. They possess noticeable anticonvulsant activity even at low concentration (25 mg/kg). Acute toxicity studies of these complexes indicate that LD{sub 50} values are greater than 1500 mg/kg and the tested animals do not show any behavioural changes.

36 MATERIALS SCIENCE↗

Agent-Based Simulation Model for Analyzing Multimodal Transportation of CO2 for CCUS

The overarching goal of this work is to determine how the United States can avoid being constrained by transportation limitations as the CCUS process evolves to a full gigaton-level system. The model is data-driven, open to CO2 supply and demand points defined as input data, and designed to allow for transportation on waterways, rail, or pipeline.

Clark, RobinJ↗

Protein abundances can distinguish between naturally-occurring and laboratory strains of Yersinia pestis , the causative agent of plague

Adaptive processes in bacterial species can occur rapidly in laboratory culture, leading to genetic divergence between naturally occurring and laboratory-adapted strains. Differentiating wild and closely-related laboratory strains is clearly important for biodefense and bioforensics; however, DNA sequence data alone has thus far not provided a clear signature, perhaps due to lack of understanding of how diverse genome changes lead to adapted phenotypes. Protein abundance profiles from mass spectrometry-based proteomics analyses are a molecular measure of phenotype. Proteomics data contains sufficient information that powerful statistical methods can uncover signatures that distinguish wild strains of Yersinia pestis from laboratory-adapted strains.

59 BASIC BIOLOGICAL SCIENCES↗

Autoclave treatment of the classical scrapie agent US No. 13-7 and experimental inoculation to susceptible VRQ/ARQ sheep via the oral route results in decreased transmission efficiency

Scrapie, a prion disease of sheep, is highly resistant to conventional deactivation. Numerous methods to deactivate scrapie have been tested in laboratory animal models, and adequate autoclave treatment can reduce or remove the infectivity of some classical scrapie strains depending on the heating parameters used. In this study, we autoclaved brain homogenate from a sheep with US scrapie strain 13–7 for 30 minutes at 121°C. Genetically susceptible VRQ/ARQ sheep were orally inoculated with 3 grams of the autoclaved brain homogenate. For comparison, a second group of sheep was inoculated with a non-autoclaved brain homogenate. Rectal biopsies were used to assess antemortem scrapie disease progression throughout the study. Five out of ten (5/10) sheep that received autoclaved inoculum ultimately developed scrapie after an experimental endpoint of 72 months. These sheep had a mean incubation period of 26.99 months. Two out of five (2/5) positive sheep had detectable PrP Sc in antemortem rectal biopsies, and two (2/5) other sheep had PrP Sc in postmortem rectal tissue. A single sheep (1/5) was positive for scrapie in the CNS, small intestine, and retropharyngeal lymph node but had negative rectal tissue. All of the sheep (10/10) that received non-autoclaved inoculum developed scrapie with a mean incubation period of 20.2 months and had positive rectal biopsies at the earliest timepoint (14.7 months post-inoculation). These results demonstrate that sheep are orally susceptible to US derived classical scrapie strain 13–7 after autoclave treatment at 121°C for 30 minutes. Differences in incubation periods and time interval to first positive rectal biopsies indicate a partial reduction in infectivity titers for the autoclaved inoculum group.

59 BASIC BIOLOGICAL SCIENCES↗

Temporal serum neurofilament light chain concentrations in sheep inoculated with the agent of classical scrapie

Objective: Neurofilament light chain (Nf-L) has been used to detect neuroaxonal damage in the brain caused by physical injury or disease. The purpose of this study was to determine if serum Nf-L could be used as a biomarker for pre-symptomatic detection of scrapie in sheep. Methods: Four sheep with prion protein genotype AVQQ were intranasally inoculated with the classical scrapie strain x124. Blood was collected every 4 weeks until 44 weeks post-inoculation, at which point weekly collection commenced. Serum was analyzed using single molecule array (Quanterix SR-X) to evaluate Nf-L concentrations. Results: Scrapie was confirmed in each sheep by testing homogenized brainstem at the level of the obex with a commercially available enzyme immunoassay. Increased serum Nf-L concentrations were identified above the determined cutoff during the last tenth of the respective incubation period for each sheep. Throughout the time course study, PrP Sc accumulation was not detected antemortem by immunohistochemistry in rectal tissue at any timepoint for any sheep. RT-QuIC results were inconsistently positive throughout the timepoints tested for each sheep; however, each sheep had at least one timepoint detected positive. When assessing serum Nf-L utility using receiver operator characteristic curves against different clinical parameters, such as asymptomatic and symptomatic (pruritus or neurologic signs), results showed that Nf-L was most useful at being an indicator of disease only late in disease progression when neurologic signs were present. Conclusion: Serum Nf-L concentrations in the cohort of sheep increased as disease progressed; however, serum Nf-L did not increase during the presymptomatic window. The levels increased substantially throughout the final 10% of the animals’ scrapie incubation period when other clinical signs were present. Serum Nf-L is not a reliable biomarker for pre-clinical detection of scrapie.

59 BASIC BIOLOGICAL SCIENCES↗

Direct Injection of Biomineralizing Agents to Restore Injectivity and Wellbore Integrity

Summary In this manuscript, we describe the second of two field demonstrations of microbially induced calcium carbonate precipitation (MICP) performed in a failed waterflood injection well in Indiana. In 2012, fracture-related flow pathways developed in the wellbore cement, causing injection water to bypass the oil-bearing formation and enter a high-permeability sandstone thief zone, thereby substantially decreasing injection pressure. In the first field demonstration, our study team characterized the well's mode of failure and successfully applied MICP to decrease flow through the defective cement. However, because the MICP treatment was conducted using a bailer delivery system, the degree of permeability reduction achievable was not adequate to fully restore the historic injection pressure of 1,400 psi at 1 gal/min. For the second field demonstration (reported herein), a direct injection system was developed that substantially increased the injection volume of MICP-promoting fluids. Two strategies were implemented to produce more ureolytic microbes: resuspending concentrated frozen cells immediately before injection and scaling up the bioreactor growth capacity. Multiple pulses of microbes and urea-calcium media were pumped into a string of 1-in.-diameter tubing separated by brine spacers and injected continuously at a flow rate of 3.4 to 1.4 gal/min. During the third day of injection, an injection pressure of 1,384 psi at a flow rate of 1.4 gal/min was achieved, and the experiment was terminated. This study demonstrates that MICP can be successfully used in large-volume applications where the time frame for the delivery of reactants is limited. This finding has significant relevance for commercialization of the MICP biotechnology in the oil and gas industry.

Engineering↗

Real-Time Monitoring of Fracture Dynamics with a Contrast Agent-Assisted Electromagnetic Method

In collaboration with the Advanced Energy Consortium, our team has previously demonstrated that the placement of electrically active proppants (EAPs) in a hydraulic fracture surveyed by electromagnetic (EM) methods can enhance the imaging of the stimulated reservoir volumes during hydraulic fracturing. That work culminated in constructing a well-characterized EAP-filled fracture anomaly at the Devine field pilot site (DFPS). In subsequent laboratory studies, we observed that the electrical conductivity of our EAP correlates with changes in pressure, salinity, and flow. Thus, we postulated that the EAP could be used as an in-situ sensor for the remote monitoring of these changes in previously EAP-filled fractures. This paper presents our latest field data from the DFPS to demonstrate such correlations at an intermediate pilot scale. We conducted surface-based EM surveys during freshwater (200 ppm) and saltwater (2,500 ppm) slug injections while running surfaced-based EM surveys. Simultaneously, we measured the following: 1) bottomhole pressure and salinity in five monitoring wells; 2) injection rate using high-precision data loggers; 3) distributed acoustic sensors in four monitoring wells; and 4) tiltmeter data on the survey area. We demonstrated that injections into an EAP-filled fracture could be successfully coupled with real-time electric field measurements on the surface, leading to remote monitoring of dynamic changes within the EAP-filled fracture. Furthermore, by comparing the electrical field traces with the bottomhole pressure, flow rate, and salinity, we concluded that the observed electric field in our study is influenced by fracture dilation and flow rate. Salinity effect was observed when saltwater was injected. EM simulations solely based on assumptions of fracture conductivity changes during injection did not reproduce all of the measured electric field magnitudes. Preliminary estimates showed that including streaming potential in our geophysical model may be needed to reduce the simulation mismatch. The methods developed and demonstrated during this study will lead to a better understanding of the extent of fracture networks, formation stress states, fluid leakoff and invasion, characterizations of engineered fracture systems, and other applications where monitoring subsurface flow tracking is deemed important.

02 PETROLEUM↗

Critical cleaning agents for Di-2-ethylhexyl sebacate.

It is required that Di-2-ethylhexyl Sebacate oil, also commonly known as Dioctyl Sebacate oil, be thoroughly removed from certain metals, in this case stainless steel parts with narrow, enclosed spaces. Dioctyl Sebacate oil is a synthetic oil with a low compressibility. As such, it is ideally used for high pressure calibrations. The current method to remove the Dioctyl Sebacate from stainless steel parts with narrow, enclosed spaces is a labor-intensive, multi-step process, including a detergent clean, a deionized (DI) water rinse, and several solvent rinses, to achieve a nonvolatile residue of 0.04 mg per 50 mL rinse effluent. This study was undertaken to determine a superior detergent/solvent cleaning method for the oil to reduce cleaning time and/or the amount of detergent/solvent used. It was determined that while some detergent clean the oil off the metal better than the current procedure, using only solvents obtained the best result. In addition, it can be inferred, based on elevated temperature test results, that raising the temperature of the oil-contaminated stainless steel parts to approximately 50ÀC will provide for improved cleaning efficacy.

Hartley, Mya↗