Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “SAMPLE PREPARATION”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 973 records · Page 54
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Torsional force microscopy of van der Waals moirés and atomic lattices

In a stack of atomically thin van der Waals layers, introducing interlayer twist creates a moiré superlattice whose period is a function of twist angle. Changes in that twist angle of even hundredths of a degree can dramatically transform the system’s electronic properties. Setting a precise and uniform twist angle for a stack remains difficult; hence, determining that twist angle and mapping its spatial variation is very important. Techniques have emerged to do this by imaging the moiré, but most of these require sophisticated infrastructure, time-consuming sample preparation beyond stack synthesis, or both. In this work, we show that torsional force microscopy (TFM), a scanning probe technique sensitive to dynamic friction, can reveal surface and shallow subsurface structure of van der Waals stacks on multiple length scales: the moirés formed between bi-layers of graphene and between graphene and hexagonal boron nitride (hBN) and also the atomic crystal lattices of graphene and hBN. In TFM, torsional motion of an Atomic Force Microscope (AFM) cantilever is monitored as it is actively driven at a torsional resonance while a feedback loop maintains contact at a set force with the sample surface. TFM works at room temperature in air, with no need for an electrical bias between the tip and the sample, making it applicable to a wide array of samples. It should enable determination of precise structural information including twist angles and strain in moiré superlattices and crystallographic orientation of van der Waals flakes to support predictable moiré heterostructure fabrication.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS1995

Inflight resistance measurement on high-T(sub c) superconducting thin films exposed to orbital atomic oxygen on CONCAP-2 (STS-46)

In 1992, UAH (University of Alabama in Huntsville) conducted a unique experiment on STS-46 in which YBa2Cu3O7 (commonly known as '1-2-3' superconductor) high-T(c) superconducting thin film samples prepared at three different laboratories were exposed to 5 eV atomic oxygen in low Earth orbit on the ambient and 320 C hot plate during the first flight of the CONCAP-2 (Complex Autonomous Payload) experiment carrier. The resistance of the thin films was measured in flight during the atomic oxygen exposure and heating cycle. Superconducting properties were measured in the laboratory before and after the flight by the individual experimenters. Films with good superconducting properties, and which were exposed to the oxygen flux, survived the flight including those heated to 320 C (600 K) with properties essentially unchanged, while other samples which were heated but not exposed to oxygen were degraded. The properties of other flight controls held at ambient temperature appear unchanged and indistinguishable from those of ground controls, whether exposed to oxygen or not.

Gregory, J. C.↗
DOE OSTI2025

OzMALDI: A Gas-Phase, In-Source Ozonolysis Reaction for Efficient Double-Bond Assignment in Mass Spectrometry Imaging with Matrix-Assisted Laser Desorption/Ionization

Lipids make up an important class of biomolecules with diverse structures and varied chemical functions. This diversity is a major challenge in chemical analysis and limits our understanding of biological functions and regulation. A major way lipid isomers differ is by double-bond (db) position, and analyzing db-isomers is especially challenging for mass spectrometry imaging (MSI). Ozonolysis can be used to determine the dbposition and has been paired with MSI before. However, previous techniques require increased analysis time to allow for gas-phase reactions within an ion trap or ion mobility cell or additional sample preparation time to allow for offline ozonation. Here, we introduce a new ozonolysis method inside the matrix-assisted laser desorption-ionization (MALDI) source, termed OzMALDI, that simultaneously produces ozonides from all unsaturated lipids. This allows us to determine db-positions without adding additional reaction time while maintaining the high mass resolution provided by Orbitrap MS. This new technique is especially effective at determining multiple db-positions in lipids containing polyunsaturated fatty acids, which is a limitation of many previous techniques. OzMALDI-MSI was applied to the analysis of rat brain and genetically engineered Camelina and soybean seed samples, demonstrating the utility of this method and uncovering novel biological information.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Probing Microstructure-induced Swelling & Thermal Property Changes in Ion-Irradiated Oxide Fuels using Laser-generated Surface Acoustic Waves

Radiation of fuel rods with neutrons during a fission reaction in a nuclear reactor is known to affect the material microstructure of the fuel as a result of fission fragment damage, and lead to the formation of atomic-level defects such as voids, dislocation loops, and lattice swelling from fission-gas release. A consequence of the radiation-induced damage in nuclear fuels is the drastic alteration of material properties, in particular, the reduction of the thermal conductivity – a key parameter that governs the transport of thermal energy released from fissile fuel atoms to the surrounding coolant. Swelling can induce high stresses and ultimate failure of the cladding. A fundamental understanding of the role of radiation-induced damage on the thermal transport and mechanical properties of nuclear fuels is therefore critical for efficient, reliable and safe operation of a nuclear power plant. As opposed to conventional post-irradiation examination techniques that are often time-consuming and require significant sample preparation, laser-based characterization methods have emerged as promising non-contact, non-destructive tools to measure the evolution of microstructure-induced material property changes. Moreover, laser methods offer the promise of in-situ characterization while the material is being irradiated. This project aims to develop an improved understanding of the impact of radiation-induced changes to material microstructure on the thermal and elastic properties of nuclear materials. A laser ultrasonic technique, known as the transient grating (TG) spectroscopy method, is used to simultaneously measure thermal diffusivity and elastic properties in unirradiated and ion-irradiated oxide nuclear fuel samples. The results will complement on-going investigations on electron- and phonon-mediated thermal transport in nuclear materials and will provide foundational work for incorporating the influence of defects in fuel performance codes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Steady-state and time-resolved Thioflavin-T fluorescence can report on morphological differences in amyloid fibrils formed by Aβ(1-40) and Aβ(1-42)

Thioflavin-T (ThT) is one of the most commonly used dyes for amyloid detection, but the origin of its fluorescence enhancement is not fully understood. Herein we have characterised the ThT fluorescence response upon binding to the Aβ(1-40) and Aβ(1-42) variants of the Alzheimer's-related peptide amyloid-β, in order to explore how the photophysical properties of this dye relates to structural and morphological properties of two amyloid fibril types formed by peptides with a high degree of sequence homology. We show that the steady-state ThT fluorescence is 1.7 times more intense with Aβ(1-40) compared to Aβ(1-42) fibrils in concentration matched samples prepared under quiescent conditions. By measuring the excited state lifetime of bound ThT, we also demonstrate a distinct difference between the two fibril isoforms, with Aβ(1-42) fibrils producing a longer ThT fluorescence lifetime compared to Aβ(1-40). The substantial steady-state intensity difference is therefore not explained by differences in fluorescence quantum yield. Further, we find that the ThT fluorescence intensity, but not the fluorescence lifetime, is dependent on the fibril preparation method (quiescent versus agitated conditions). We therefore propose that the fluorescence lifetime is inherent to each isoform and sensitively reports on fibril microstructure in the protofilament whereas the total fluorescence intensity relates to the amount of exposed β-sheet in the mature Aβ fibrils and hence to differences in their morphology. Our results highlight the complexity of ThT fluorescence, and demonstrate its extended use in amyloid fibril characterisation. - Highlights: • ThT emission is more intense with Aβ(1-40) fibrils than with Aβ(1-42) fibrils. • Aβ(1-42) fibrils induce longer ThT fluorescence lifetimes and higher quantum yield. • ThT emission intensity in Aβ fibril samples reports on fibril morphology. • The ThT fluorescence lifetime is a characteristic feature of each Aβ fibril type.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Rapid Nucleic Acid Extraction and Purification Using a Miniature Ultrasonic Technique

Miniature ultrasonic lysis for biological sample preparation is a promising technique for efficient and rapid extraction of nucleic acids and proteins from a wide variety of biological sources. Acoustic methods achieve rapid, unbiased, and efficacious disruption of cellular membranes while avoiding the use of harsh chemicals and enzymes, which interfere with detection assays. In this work, a miniature acoustic nucleic acid extraction system is presented. Using a miniature bulk acoustic wave (BAW) transducer array based on 36° Y-cut lithium niobate, acoustic waves were coupled into disposable laminate-based microfluidic cartridges. To verify the lysing effectiveness, the amount of liberated ATP and the cell viability were measured and compared to untreated samples. The relationship between input power, energy dose, flow-rate, and lysing efficiency were determined. DNA was purified on-chip using three approaches implemented in the cartridges: a silica-based sol-gel silica-bead filled microchannel, nucleic acid binding magnetic beads, and Nafion-coated electrodes. Using E. coli, the lysing dose defined as ATP released per joule was 2.2× greater, releasing 6.1× more ATP for the miniature BAW array compared to a bench-top acoustic lysis system. An electric field-based nucleic acid purification approach using Nafion films yielded an extraction efficiency of 69.2% in 10 min for 50 µL samples.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2012

Analysis of Chloroquine and Metabolites Directly from Whole-body Animal Tissue Sections by Liquid Extraction Surface Analysis (LESA) and Tandem Mass Spectrometry

The rapid and direct analysis of the amount and spatial distribution of exogenous chloroquine and chloroquine metabolites from tissue sections by liquid extraction surface sampling analysis coupled with tandem mass spectrometry (LESA-MS) was demonstrated. LESA-MS results compared well with previously published chloroquine quantification data collected by organ excision, extraction and fluorescent detection. The ability to directly sample and analyze spatially-resolved exogenous molecules from tissue sections with minimal sample preparation and analytical method development has the potential to facilitate the assessment of target tissue penetration of pharmaceutical compounds, to establish pharmacokinetic/pharmacodynamic (PK/PD) relationships, and to complement established pharmacokinetic methods used in the drug discovery process during tissue distribution assessment.

chloroquine↗
DOE OSTI2020

Synthesis routes to eliminate oxide impurity segregation and their influence on intergrain connectivity in K-doped BaFe 2 As 2 polycrystalline bulks

The poor reproducibility of intergrain critical current density $J_c$ in Fe-based superconductors is often believed to result from uncontrolled grain boundary (GB) connectivity degraded by extrinsic factors such as the local or global impurity concentration or GB porosity or cracks. Earlier we found that Ba and K can appear as oxide impurities at GBs, along with GB-wetting FeAs. In this study, we evaluated how the sample preparation environment and purity of the starting materials influence the polycrystalline $J_c$ in K-doped BaFe 2 As 2 (Ba122) bulks. Using a high-performance glovebox, the oxygen and water levels were significantly reduced, eliminating traces of FeAs. We report oxide impurities and Ba (or K) segregation associated with oxygen in the starting materials were significantly reduced by using high purity starting materials. This combination essentially doubled the best $J_c$(4.2 K) values to 2.3 × 10 5 at self-field and 1.6 × 10 4 A cm –2 at 10 T and analytical scanning transmission electron microscopy showed no GB or O segregation in the best samples, but did show dark Z-contrast and distinct nanoscale porosity. Our work shows that an inert synthesis environment and high purity K and Ba do reduce current-blocking oxygen impurity and GB impurity phases, allowing deeper exploration of the role of extrinsic and intrinsic GB blocking effects in controlling the $J_c$ of polycrystalline Ba122.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Cast Stone Oxidation Front Evaluation: Preliminary Results For Samples Exposed To Moist Air

The rate of oxidation is important to the long-term performance of reducing salt waste forms because the solubility of some contaminants, e.g., technetium, is a function of oxidation state. TcO 4 - in the salt solution is reduced to Tc(IV) and has been shown to react with ingredients in the waste form to precipitate low solubility sulfide and/or oxide phases. Upon exposure to oxygen, the compounds containing Tc(IV) oxidize to the pertechnetate ion, Tc(VII)O 4 - , which is very soluble. Consequently the rate of technetium oxidation front advancement into a monolith and the technetium leaching profile as a function of depth from an exposed surface are important to waste form performance and ground water concentration predictions. An approach for measuring contaminant oxidation rate (effective contaminant specific oxidation rate) based on leaching of select contaminants of concern is described in this report. In addition, the relationship between reduction capacity and contaminant oxidation is addressed. Chromate (Cr(VI) was used as a non-radioactive surrogate for pertechnetate, Tc(VII), in Cast Stone samples prepared with 5 M Simulant. Cast Stone spiked with pertechnetate was also prepared and tested. Depth discrete subsamples spiked with Cr were cut from Cast Stone exposed to Savannah River Site (SRS) outdoor ambient temperature fluctuations and moist air. Depth discrete subsamples spiked with Tc-99 were cut from Cast Stone exposed to laboratory ambient temperature fluctuations and moist air. Similar conditions are expected to be encountered in the Cast Stone curing container. The leachability of Cr and Tc-99 and the reduction capacities, measured by the Angus-Glasser method, were determined for each subsample as a function of depth from the exposed surface. The results obtained to date were focused on continued method development and are preliminary and apply to the sample composition and curing / exposure conditions described in this report. The Cr oxidation front (depth to which soluble Cr was detected) for the Cast Stone sample exposed for 68 days to ambient outdoor temperatures and humid air (total age of sample was 131 days) was determined to be about 35 mm below the top sample surface exposed. The Tc oxidation front, depth at which Tc was insoluble, was not determined. Interpretation of the results indicates that the oxidation front is at least 38 mm below the exposed surface. The sample used for this measurement was exposed to ambient laboratory conditions and humid air for 50 days. The total age of the sample was 98 days. Technetium appears to be more easily oxidized than Cr in the Cast Stone matrix. The oxidized forms of Tc and Cr are soluble and therefore leachable. Longer exposure times are required for both the Cr and Tc spiked samples to better interpret the rate of oxidation. Tc spiked subsamples need to be taken further from the exposed surface to better define and interpret the leachable Tc profile. Finally Tc(VII) reduction to Tc(IV) appears to occur relatively fast. Results demonstrated that about 95 percent of the Tc(VII) was reduced to Tc(IV) during the setting and very early stage setting for a Cast Stone sample cured 10 days. Additional testing at longer curing times is required to determine whether additional time is required to reduce 100 % of the Tc(VII) in Cast Stone or whether the Tc loading exceeded the ability of the waste form to reduce 100 % of the Tc(VII). Additional testing is required for samples cured for longer times. Depth discrete subsampling in a nitrogen glove box is also required to determine whether the 5 percent Tc extracted from the subsamples was the result of the sampling process which took place in air. Reduction capacity measurements (per the Angus-Glasser method) performed on depth discrete samples could not be correlated with the amount of chromium or technetium leached from the depth discrete subsamples or with the oxidation front inferred from soluble chromium and technetium (i.e., effective Cr and Tc oxidation fronts). Residual reduction capacity in the oxidized region of the test samples indicates that the remaining reduction capacity is not effective in re-reducing Cr(VI) or Tc(VII) in the presence of oxygen. Depth discrete sampling and leaching is a useful for evaluating Cast Stone and other chemically reducing waste forms containing ground granulated blast furnace slag (GGBFS) or other reduction / sequestration reagents to control redox sensitive contaminant chemistry and leachability in the near surface disposal environment. Based on results presented in this report, reduction capacity measured by the Angus-Glasser Ce(IV) method is not an appropriate or meaningful parameter for determining or predicting Tc and Cr oxidation / retentions, speciation, or solubilities in cementitious materials such as Cast Stone. A model for predicting Tc(IV) oxidation to soluble Tc(VII) should consider the waste form porosity (pathway for oxygen ingress), oxygen source, and the contaminant specific oxidation rates and oxidation fronts. Depth discrete sampling of materials exposed to realistic conditions in combination with short term leaching of crushed samples has potential for advancing the understanding of factors influencing performance. This information can be used to support conceptual model development.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Temperature dependent dielectric and magnetic properties of GdFe{sub 1−x}Ni{sub x}O{sub 3} (0.0 ≤ x ≤ 0.3) orthoferrites

The polycrystalline samples of GdFe{sub 1−x}Ni{sub x}O{sub 3} (x = 0.0, 0.1, 0.2, 0.3) orthoferrites are synthesized via solid state reaction route. The Rietveld fitted X-ray diffraction patterns confirm the formation of orthorhombic phase with Pbnm space group for all the samples. The dielectric measurements reveal an enhancement in dielectric constant and tangent loss with increase in both temperature as well as Nickel (Ni) substitution. Dielectric studies are also in support with the induction of delocalized charge carriers in the GdFeO{sub 3} matrix with increasing Ni doping. Magnetization versus applied field study shows the non-saturating hysteresis curves suggesting the canted type antiferromagnetic behavior in the considered orthoferrites. Moreover, the observed magnetic behavior is complex and the doping affects the magnitude of magnetization differently at 300 K and 80 K. It has further been noticed that the incorporated Ni{sup 3+} ions enhances the symmetry of the magnetization curves. The as-prepared samples may find their applications in the decoupling capacitors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Crystallographic orientation of uniaxial calcite and dolomite determined using reflection generalized ellipsometry

In this study, using the two-modulator generalized ellipsometry microscope (2-MGEM), it is shown that it is possible to determine the direction of the optic axis of crystallites of the high birefringence materials calcite and dolomite. 2-MGEM measurements are performed in reflection at near-normal incidence, so sample preparation requires only an optically polished surface. For uniaxial materials, the 2-MGEM measures the direction of the fast axis and the diattenuation, which can then be related to the tilt angle of the optic axis with respect to the surface normal once the maximum diattenuation is known. The optical resolution of the present instrument is 4-6 μm, and areas as large as 1 cm 2 can be measured without distortion. Additionally, the 2-MGEM measures the depolarization, which is a measure of the quality of the data. Using this information, an optical pole figure can be determined. The 2-MGEM results are compared with electron backscatter diffraction (EBSD) measurements on the same samples. Lastly, additional standard spectroscopic generalized ellipsometry measurements at a large angle of incidence were performed on single crystal calcite and dolomite to determine the spectroscopic ordinary and extraordinary refractive indices from 220 nm to 850 nm from which the maximum diattenuation can be determined.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Using X-ray Micro-Computed Tomography to Three-Dimensionally Visualize the Foregut of the Glassy-Winged Sharpshooter ( Homalodisca vitripennis )

Dissecting the heads of small insects belonging to the order Hemiptera for detailed anatomical investigation with light or scanning electron microscopy is difficult, time-consuming, and destructive, often resulting in sample preparation artifacts. Nevertheless, the structural details of these insects often hold critical information regarding their interactions with bacterial pathogens. For example, the glassy-winged sharpshooter (GWSS) is an efficient vector of the bacterium Xylella fastidiosa, the causal agent of Pierce’s disease in grape vines, but the foregut of this species is exceptionally difficult to dissect. Here, we describe a simple, non-destructive method to investigate the structure of the anterior gut of GWSS using high-resolution micro-computed X-ray tomography (microCT). The use of microCT eliminates the need for destructive dissection and reveals the morphology of small insects in three dimensions, allowing the user to virtually dissect the sample. The use of microCT imaging is a promising and powerful tool in the entomological sciences for studying the structures of vector insects, especially for difficult-to-dissect regions such as the foregut.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2016

A Simple and Sensitive LC-MS/MS Method for the Determination of Free 8-Hydroxy-2'-Deoxyguanosine in Human Urine

Urinary free 8-hydroxy-2'-deoxyguanosine (8OHdG), an oxidized product of DNA, and is frequently chosen as a biomarker of oxidative stress in humans, including studies of oxidative DNA damage during space flight. It is challenging to accurately and efficiently quantify urinary free 8OHdG in large scale human studies. LC-MS/MS is emerging as a preferable analytical technique owing its high sensitivity, selectivity and efficiency, compared to some traditional methods such as ELISA and HPLC. A simple and sensitive LC-MS/MS method has been developed for the determination of free 8OHdG in human urine. Sample preparation was done by solid phase extraction with a Waters Oasis HLB 96 well plate. A Waters Alliance 2795 HT Separation Module combined with a Quattro Micro tandem mass spectrometer was used as the LC-MS/MS system. The runtime of one injection can be less than 5 minutes using a reversed phase C18 column and an isocratic flow of methanol/water. ESI positive ions were quantified in the multiple reaction modes (MRM) using m/z 284 yields 168 for 8OHdG and m/z 289 yields173 for stable isotope labeled internal standard [(15)N5] 8OHdG. With this method for 8OHdG, a lower limit of quantitation of 1.0 nM (0.28 ng/mL) has been achieved using 100 microliter urine sample. The analytical range is between 1.0 and 100 nM with a correlation coefficient greater than or equal to 0.99. Good reproducibility can be obtained with intra-assay and inter-assay CVs less than or equal to 10% for 8OHdG spiked urine QC samples. This method can be used in high-throughput routine analysis of free 8OHdG in human urine.

Wang, Zuwei↗
DOE OSTI2013

Optical and electrochemical studies of polyaniline/SnO{sub 2} fibrous nanocomposites

Graphical abstract: Fiber with porous like structure of PANI/SnO{sub 2} nanocomposites were prepared by simplest in situ chemical polymerization method. The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The excellent electrochemical properties of composite electrode show the specific capacitance of 173 F/g at a scan rate of 25 m V/s. Display Omitted Highlights: ► Self assembled PANI/SnO{sub 2} nanocomposites were synthesized by simple polymerization method. ► Electrochemical behavior of PANI/SnO{sub 2} nanocomposites electrode was analyzed by CV. ► Nanocomposites exhibit a higher specific capacitance of 173 F/g, compared with pure SnO{sub 2}. -- Abstract: Polyaniline (PANI)/tin oxide (SnO{sub 2}) fibrous nanocomposites were successfully prepared by an in situ chemical polymerization method with suitable conditions. The obtained composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy, photoluminescence (PL), electrical conductivity and cyclic voltammetry studies (CV). The XRD pattern of the as-prepared sample shows the presence of tetragonal SnO{sub 2} and the crystalline structure of SnO{sub 2} was not affected with the incorporation of PANI. The FTIR analysis confirms the uniform attachment of PANI on the surface of SnO{sub 2} nanostructures. SEM images show a fibrous agglomerated structure of PANI/SnO{sub 2}. The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The electrochemical behavior of the PANI/SnO{sub 2} composite electrode was evaluated in a H{sub 2}SO{sub 4} solution using cyclic voltammetry. The composite electrode exhibited a specific capacitance of 173 F/g at a scan rate 25 mV/s. Thus the as-prepared PANI/SnO{sub 2} composite shows excellent electrochemical properties, suggesting that this composite is a promising material for supercapacitors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

The AMWCNTs supported porous nanocarbon composites for high-performance supercapacitor

Graphical abstract: The AMWCNTs supported porous nanocarbon composites were prepared by a easy method. The composites had shown good performances for electrochemical energy storage with high specific capacitance and good stability. - Highlights: • The AMWCNTs supported porous nanocarbon composites were prepared. • The composites have good conductivity and large BET specific surface areas. • The composites had shown high specific capacitance, and good stability. - Abstract: The porous nanocarbons supported by acid-treated multiwall carbon nanotubes (PC@ACNTs) were prepared by the combination of the hydrothermal polymerization of glucose on ACNTs, carbonization under N{sub 2} protection and final activation with ZnCl{sub 2}. The materials were characterized by transmission electron microscopy, X-ray powder diffraction and Raman spectra. The results indicated that the ACNTs distributed uniformly into the framework of the porous carbon. The composites showed the high BET specific surface area up to 1712 m{sup 2} g{sup −1} and good conductivity. The electrochemical measurements indicated that the composites processed good performances for electrochemical energy storage (210 F g{sup −1} at 0.5 A g{sup −1}), and high stability (>99.9%), much higher than the corresponding ACNTs, porous carbons and the samples prepared by using raw MWCNTs as source. The good performance of PC@ACNTs composites was relative with the synergy of good conductivity of ACNTs and large specific surface areas of PC.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Development of Nontargeted Workflow of Occupational Exposure by Infrared Ion Spectroscopy and Silicone Wristbands’ Passive Sampling

Monitoring chemical exposure has well-established protocols and procedures for occupational health and industrial hygiene across various career fields and in a variety of occupational and environmental conditions. Iterative analytical development has led to validated methods to provide employers and employees with safe working conditions in terms of industrial hygiene. These validated methods are commonly supported by commercial laboratories. Here, this workflow is explicitly a targeted approach in which sampling media, sample preparation, chemical separation, quantitative target detection, and post processing are well established. This workflow also relies on commercially available chemical surrogates, isotopically labeled internal standards, and certified/standard reference materials from reputable vendors. An untargeted workflow lacks many key ingredients of validated analytical methods to include the known chemical target.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

A New One-Pot Sequential Reduction-Deposition Method for the synthesis of Silica-supported NiPt and CuPt Bimetallic Catalysts

A one-pot redox deposition method is described to prepare silica-supported bimetallic NiPt and CuPt catalysts using differences in standard reduction potentials. The synthesis involved the initial reduction of non-noble metal ions (Ni 2+ and Cu 2+ ) by NaBH 4 , followed by reduction of Pt ions by these reduced metals. Alloy formation and phase purity were established by X-ray diffraction (XRD), bulk composition by X-ray fluorescence (XRF), and surface composition by X-ray photoelectron spectroscopy (XPS). Alloy formation was enhanced by increase in the amount of base metals available to reduce Pt, or through the use of excess NaBH 4 after redox deposition. The catalysts were evaluated for methane oxidation at 300-400 °C and atmospheric pressure. Reference samples prepared using the incipient wetness impregnation (IW) method had inferior performance and characteristics. The redox deposition method provides a simple and versatile protocol for the preparation of bimetallic alloys between noble metals and base metals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Preparation of a new pyrochlore-type compound Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46}(OH){sub 0.44} by hydrothermal reaction

A new pyrochlore-type Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46}(OH){sub 0.44} with the cubic cell of a=10.339(5) A was prepared by hydrothermal reaction using TiO{sub 2} (anatase) and Bi{sub 2}O{sub 3} in NaOH solution. This compound was obtained when the molar ratio of NaOH/TiO{sub 2} was above 2 and the reaction temperature was above 240 deg. C. The TG-curve of as-prepared sample showed a mass loss of 0.8 mass% which was caused by release of OH group. This compound decomposed to a pyrochlore-type compound and a layered-type Na{sub 0.5}Bi{sub 4.5}Ti{sub 4}O{sub 15} above 800 deg. C. The optical band gap of Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46}(OH){sub 0.44} was estimated to be 2.5 eV. - Graphical abstract: SEM image and schematic representation of the structure of Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46} (OH){sub 0.44}. Highlights: > A new pyrochlore-type Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46}(OH){sub 0.44} is first prepared via a facile hydrothermal route. > The chemical composition is concluded to be Na{sub 0.32}Bi{sub 1.68}Ti{sub 2}O{sub 6.46}(OH){sub 0.44} from the analysis of experimental results. > The crystal data and atomic parameters can compare with those of pyrochlore-type bismuth titanates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗