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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.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Evaluation of surface sampling method performance for Bacillus Spores on clean and dirty outdoor surfaces.

Recovery of Bacillus atrophaeous spores from grime-treated and clean surfaces was measured in a controlled chamber study to assess sampling method performance. Outdoor surfaces investigated by wipe and vacuum sampling methods included stainless steel, glass, marble and concrete. Bacillus atrophaeous spores were used as a surrogate for Bacillus anthracis spores in this study designed to assess whether grime-coated surfaces significantly affected surface sampling method performance when compared to clean surfaces. A series of chamber tests were carried out in which known amounts of spores were allowed to gravitationally settle onto both clean and dirty surfaces. Reference coupons were co-located with test coupons in all chamber experiments to provide a quantitative measure of initial surface concentrations of spores on all surfaces, thereby allowing sampling recovery calculations. Results from these tests, carried out under both low and high humidity conditions, show that spore recovery from grime-coated surfaces is the same as or better than spore recovery from clean surfaces. Statistically significant differences between method performance for grime-coated and clean surfaces were observed in only about half of the chamber tests conducted.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In Situ Chemical Monitoring and Imaging of Contents within Microfluidic Devices Having a Porous Membrane Wall Using Liquid Microjunction Surface Sampling Probe Mass Spectrometry

The ability to observe dynamic chemical processes (e.g., signaling, transport, etc.) in vivo or in situ using nondestructive chemical imaging opens a new door to understanding the complex dynamics of developing biological systems. With the advent of “biology-on-a-chip” devices has come the ability to monitor dynamic chemical processes in a controlled environment, using these engineered habitats to capture key features of natural systems while allowing visual observation of system development. Having the capability to spatially and temporally map the chemical signals within these devices may yield new insights into the forces that drive biosystem development. Here, a porous membrane sealed microfluidic device was designed to allow normal microfluidic operation while enabling continuous, location specific sampling and chemical characterization by liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS). LMJ-SSP was used to extract fluids with nL-to-μL/min flow rates directly from selected areas of the microfluidic device without negatively impacting the device function. These extracts were subsequently characterized using MS. This technique was used to acquire MS images of the entirety of several multi-input microfluidic devices having different degrees of fluid mixing. LMJ-SSP MS imaging visualized the spatial distribution of chemical components within the microfluidic channels and could visualize chemical reactions occurring in the device. These microfluidic devices with a porous membrane wall are wholly compatible with the construction of biology-on-a-chip devices. This ultimately would enable correlation of biosystem physical structure with an evolving chemical environment

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Surface Sampling Techniques for the Canister Deposition Field Demonstration

This report describes plans for dust sampling and analysis for the multi-year Canister Deposition Field Demonstration. The demonstration will use three commercial 32PTH2 NUHOMS welded stainless steel storage canisters, which will be stored at an ISFSI site in Advanced Horizontal Storage Modules. One canister will be unheated; the other two will have heaters to achieve canister surface temperatures that match, to the degree possible, spent nuclear fuel (SNF) loaded canisters with heat loads of 10 kW and 40 kW. Surface sampling campaigns will take place on a yearly or bi-yearly basis. The goal of the planned dust sampling and analysis is to determine important environmental parameters that impact the potential occurrence of stress corrosion cracking on SNF dry storage canisters. Specifically, the size, morphology, and composition of the deposited dust and salt particles will be quantified, as well as the soluble salt load per unit area and the rate of deposition, as a function of canister surface temperature, location, time, and orientation. Sampling locations on the canister surface will nominally include 25 locations, corresponding to 5 circumferential locations at each of the 5 longitudinal locations. At each sampling location, a 2x2 sampling grid (containing 4 sample cells) will be painted onto the metal surface. During each sampling campaign, two samples at each sampling location will be collected, in a specific routine to measure both periodic (yearly or bi-yearly) and cumulative deposition rates. For each sample, a wet and a dry sample will be collected. Wet samples will be analyzed to determine the composition of the soluble salt fraction and to estimate salt loading per unit area. Dry samples will be analyzed to assess particle size, morphology, mineralogy, and identity (e.g. for floral/faunal fragments). The data generated by this proposed sampling plan will provide detailed information on dust and salt aerosol deposits on spent nuclear fuel canister surfaces. The anticipated results include information regarding particle compositions, size distributions, and morphologies, in addition to particle deposition rates as a function of canister surface location, orientation, time, and temperature. The information gathered during the Canister Deposition Field Demonstration is critical for ongoing efforts to develop a detailed understanding of the potential for stress corrosion cracking on SNF dry storage canisters

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2012

HPTLC Plate Blotting for Liquid Microjunction Surface Sampling Probe Mass Spectrometric Analysis of Analytes Separated on a Wettable Phase Plate

A blotting method that transfers analytes separated on wettable HPTLC plates to a hydrophobic reversed-phase C8 HPLTC plate suitable for analysis with a liquid microjunction surface sampling probe electrospray ionization mass spectrometry system was described and demonstrated. The simple blotting procedure transfers the analyte from the wettable plate to the topmost surface of a rigidly backed, easy-to-mount hydrophobic substrate that already has been proven viable for analysis by this sampling probe/mass spectrometry system. The utility of the approach was demonstrated by the analysis of a four-component peptide mixture originally separated on a ProteoChrom HPTLC cellulose sheet and then blotted to the reversed phase HPTLC plate.

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

Molecular Surface Sampling and Chemical Imaging using Proximal Probe Thermal Desorption/Secondary Ionization Mass Spectrometry

Proximal probe thermal desorption/secondary ionization mass spectrometry was studied and applied to molecular surface sampling and chemical imaging using printed patterns on photopaper as test substrates. With the use of a circular cross section proximal probe with a tip diameter of 50 m and fixed temperature (350 C), the influence of probe-to-surface distance, lane scan spacing, and surface scan speed on signal quality and spatial resolution were studied and optimized. As a compromise between signal amplitude, signal reproducibility, and data acquisition time, a surface scan speed of 100 m/s, probe-to-paper surface distance of 5 m, and lane spacing of 10 m were used for imaging. Under those conditions the proximal probe thermal desorption/secondary ionization mass spectrometry method was able to achieve a spatial resolution of about 50 m as determined by the ability to distinguish surface patterns of known dimensions that were printed on the paper substrate. It is expected that spatial resolution and chemical image quality could be further improved by using probes of smaller cross section size and by incorporating a means to maintain a fixed optimal probe-to-surface distance real time, continuously adapting to the changing topography of the surface during a lane scan.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Liquid microjunction surface sampling of acetaminophen, terfenadine and their metabolites in thin tissue sections

The aim of this paper was to evaluate the analytical performance of a fully automated droplet-based surface-sampling system for determining the distribution of the drugs acetaminophen and terfenadine, and their metabolites, in rat thin tissue sections. The following are the results: The rank order of acetaminophen concentration observed in tissues was stomach > small intestine > liver, while the concentrations of its glucuronide and sulfate metabolites were greatest in the liver and small intestine. Terfenadine was most concentrated in the liver and kidney, while its major metabolite, fexofenadine, was found in the liver and small intestine. In conclusion, the spatial distributions of both drugs and their respective metabolites observed in this work were consistent with previous studies using radiolabeled drugs.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2015

Profiling of adrenocorticotropic hormone and arginine vasopressin in human pituitary gland and tumor thin tissue sections using droplet-based liquid-microjunction surface-sampling-HPLC–ESI-MS–MS

Described here are the results from the profiling of the proteins arginine vasopressin (AVP) and adrenocorticotropic hormone (ACTH) from normal human pituitary gland and pituitary adenoma tissue sections using a fully automated droplet-based liquid microjunction surface sampling-HPLC-ESI-MS/MS system for spatially resolved sampling, HPLC separation, and mass spectral detection. Excellent correlation was found between the protein distribution data obtained with this droplet-based liquid microjunction surface sampling-HPLC-ESI-MS/MS system and those data obtained with matrix assisted laser desorption ionization (MALDI) chemical imaging analyses of serial sections of the same tissue. The protein distributions correlated with the visible anatomic pattern of the pituitary gland. AVP was most abundant in the posterior pituitary gland region (neurohypophysis) and ATCH was dominant in the anterior pituitary gland region (adenohypophysis). The relative amounts of AVP and ACTH sampled from a series of ACTH secreting and non-secreting pituitary adenomas correlated with histopathological evaluation. ACTH was readily detected at significantly higher levels in regions of ACTH secreting adenomas and in normal anterior adenohypophysis compared to non-secreting adenoma and neurohypophysis. AVP was mostly detected in normal neurohypophysis as anticipated. This work demonstrates that a fully automated droplet-based liquid microjunction surface sampling system coupled to HPLC-ESI-MS/MS can be readily used for spatially resolved sampling, separation, detection, and semi-quantitation of physiologically-relevant peptide and protein hormones, such as AVP and ACTH, directly from human tissue. In addition, the relative simplicity, rapidity and specificity of the current methodology support the potential of this basic technology with further advancement for assisting surgical decision-making.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2012

Analyses and Comparison of Bulk and Coil Surface Samples from the DWPF Slurry Mix Evaporator

Sludge samples from the DWPF Slurry Mix Evaporator (SME) heating coil frame and coil surface were characterized to identify differences that might help identify heat transfer fouling materials. The SME steam coils have seen increased fouling leading to lower boil-up rates. Samples of the sludge were taken from the coil frame somewhat distant from the coil (bulk tank material) and from the coil surface (coil surface sample). The results of the analysis indicate the composition of the two SME samples are very similar with the exception that the coil surface sample shows ~5-10X higher mercury concentration than the bulk tank sample. Elemental analyses and x-ray diffraction results did not indicate notable differences between the two samples. The ICP-MS and Cs-137 data indicate no significant differences in the radionuclide composition of the two SME samples. Semi-volatile organic analysis revealed numerous organic molecules, these likely result from antifoaming additives. The compositions of the two SME samples also match well with the analyzed composition of the SME batch with the exception of significantly higher silicon, lithium, and boron content in the batch sample indicating the coil samples are deficient in frit relative to the SME batch composition.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2023

Structure-Driven Liquid Microjunction Surface-Sampling Probe Mass Spectrometry

The rhizosphere is the narrow region of soil surrounding the roots of plants that is influenced by root exudates, root secretions, and associated microbial communities. This region is crucial to plant growth and development and plays a critical role in nutrient uptake, disease resistance, and soil transformation. Understanding the function of exogenous compounds in the rhizosphere starts with determining the spatiotemporal distribution of these molecular components. Using liquid microjunction surface-sampling probe mass spectrometry (LMJ-SSP-MS) and microfluidic devices with attached microporous membranes enables in situ, nondisruptive, and nondestructive spatiotemporal measurement of exogenous compounds from plant roots. However, long imaging times (>2 h) can negatively affect plant heath and limit temporal studies. Here, we present a novel strategy to optimize the number and location of sampling sites on these microporous membrane-covered microfluidic devices. In conclusion, this novel, “structure-driven” sampling workflow takes into consideration the channel structure of the microfluidic device to maximize sampling from the channels and minimize acquisition time (~4× less time in some cases while providing similar chemical image accuracy), thus reducing stress on plants during in situ LMJ-SSP-MS analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

In Situ Detection of Amino Acids from Bacterial Biofilms and Plant Root Exudates by Liquid Microjunction Surface-Sampling Probe Mass Spectrometry

The plant rhizosphere is a complex and dynamic chemical environment where the exchange of molecular signals between plants, microbes, and fungi drives the development of the entire biological system. Exogenous compounds in the rhizosphere are known to affect plant-microbe organization, interactions between organisms, and ultimately, growth and survivability. The function of exogenous compounds in the rhizosphere is still under much investigation, specifically with respect to their roles in plant growth and development, the assembly of the associated microbial community, and the spatiotemporal distribution of molecular components. A major challenge for spatiotemporal measurements is developing a nondisruptive and nondestructive technique capable of analyzing the exogenous compounds contained within the environment. A methodology using liquid microjunction-surface sampling probe-mass spectrometry (LMJ-SSP-MS) and microfluidic devices with attached microporous membranes was developed for in situ, spatiotemporal measurement of amino acids (AAs) from bacterial biofilms and plant roots. Exuded arginine was measured from a living Pantoea YR 343 biofilm, which resulted in a chemical image indicative of biofilm growth within the device. Spot sampling along the roots of Populus trichocarpa with the LMJ-SSP-MS resulted in the detection of 15 AAs. Of note, variation in AA concentrations across the root system was observed, indicating that exudation is not homogeneous and may be linked to local rhizosphere architecture and different biological processes along the root.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2011

False negative rate and other performance measures of a sponge-wipe surface sampling method for low contaminant concentrations.

Recovery of spores from environmental surfaces is known to vary due to sampling methodology, techniques, spore size and characteristics, surface materials, and environmental conditions. A series of tests were performed to evaluate a new, validated sponge-wipe method. Specific factors evaluated were the effects of contaminant concentrations and surface materials on recovery efficiency (RE), false negative rate (FNR), limit of detection (LOD) - and the uncertainties of these quantities. Ceramic tile and stainless steel had the highest mean RE values (48.9 and 48.1%, respectively). Faux leather, vinyl tile, and painted wood had mean RE values of 30.3, 25.6, and 25.5, respectively, while plastic had the lowest mean RE (9.8%). Results show a roughly linear dependence of surface roughness on RE, where the smoothest surfaces have the highest mean RE values. REs were not influenced by the low spore concentrations tested (3 x 10{sup -3} to 1.86 CFU/cm{sup 2}). The FNR data were consistent with RE data, showing a trend of smoother surfaces resulting in higher REs and lower FNRs. Stainless steel generally had the lowest mean FNR (0.123) and plastic had the highest mean FNR (0.479). The LOD{sub 90} varied with surface material, from 0.015 CFU/cm{sup 2} on stainless steel up to 0.039 on plastic. Selecting sampling locations on the basis of surface roughness and using roughness to interpret spore recovery data can improve sampling. Further, FNR values, calculated as a function of concentration and surface material, can be used pre-sampling to calculate the numbers of samples for statistical sampling plans with desired performance, and post-sampling to calculate the confidence in characterization and clearance decisions.

09 BIOMASS FUELS↗
DOE OSTI2016

Improved explosive collection and detection with rationally assembled surface sampling materials

Sampling and detection of trace explosives is a key analytical process in modern transportation safety. In this work we have explored some of the fundamental analytical processes for collection and detection of trace level explosive on surfaces with the most widely utilized system, thermal desorption IMS. The performance of the standard muslin swipe material was compared with chemically modified fiberglass cloth. The fiberglass surface was modified to include phenyl functional groups. When compared to standard muslin, the phenyl functionalized fiberglass sampling material showed better analyte release from the sampling material as well as improved response and repeatability from multiple uses of the same swipe. The improved sample release of the functionalized fiberglass swipes resulted in a significant increase in sensitivity. Various physical and chemical properties were systematically explored to determine optimal performance. The results herein have relevance to improving the detection of other explosive compounds and potentially to a wide range of other chemical sampling and field detection challenges.

Explosive detection↗
DOE OSTI2019

Bulk single crystal growth and sample surface preparation of catalytic NaAu 2

Here in we have grown bulk single crystals of NaAu 2 for the first time to enable surface studies on the nature of the (111) bulk surface. This intermetallic compound exhibits surprisingly high catalytic activity for CO oxidation, a benchmark reaction. Theory predicts NaAu 2 to be the most thermodynamically stable composition in the Na-Au binary phase diagram and NaAu 2 has been seen to preferentially form in experiments containing Na and Au which supports this prediction. The (111) surface was also predicted to be the most stable and is nearly bulk-terminated making single crystal samples prepared with this crystallographic orientation a fitting choice. As a result, the crystal quality and surface composition of the metallographically prepared surface was determined by x-ray diffraction methods in addition to optical and electron microscopy.

(111) catalytic surface↗
DOE OSTI2017

Chemical Analysis of Canister Surface Samples

Electric Power Research Institute, Inc. (EPRI) and Sandia National Laboratories (SNL) collaborated to analyze dust and surface deposits on spent nuclear fuel (SNF) dry storage canisters at interim storage sites. The U.S. currently has no clear pathway for the ultimate disposition of spent fuel, so spent fuel will continue to be stored in dry casks for an extended period of time, likely well beyond the current license period of 60 years. Data on the behavior of dry storage systems and the spent fuel inside them after some period of dry storage, particularly extended storage, are limited. Potential degradation mechanisms for the canisters and fuel need to be identified and addressed for extended storage of spent fuel in dry casks past the renewal period and beyond 60 years.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Evaluating and modeling the effects of surface sampling factors on the recovery of organic chemical attribution signatures using the accelerated diffusion sampler and solvent extraction

In this study, an experimental design matrix was created and executed in order to test the effects of various real-world factors on the ability of the (1) accelerated diffusion sampler with solid phase micro-extraction (ADS-SPME) and (2) solvent extraction to capture organic chemical attribution signatures (CAS) from dimethyl methylphosphonate (DMMP) spiked onto painted wall board (PWB) surfaces. The DMMP CAS organic impurities sampled by ADS-SPME and solvent extraction were analyzed by gas chromatography/mass spectrometry (GC/MS). The number of detected DMMP CAS impurities and their respective GC/MS peak areas were determined as a function of DMMP stock, DMMP spiked volume, exposure time, SPME sampling time, and ADS headspace pressure. Based on the statistical analysis of experimental results, several general conclusions are made: (1) ADS-SPME with vacuum (i.e., reduced pressure) increased the amount of detected CAS impurity, as measured by GC/MS peak area, by a factor of 1.7 to 1.9 for PWB under certain experimental conditions, (2) the amount of detected CAS impurity was most influenced by spiked volume, stock, and ADS headspace pressure, (3) the ADS had no measurable effect on the number of detected DMMP impurities, that is, the ADS (with and without reduced pressure) had no practical effect on the DMMP impurity profile collected from spiked PWB, and (4) solvent extraction out performed ADS-SPME in terms of consistently capturing all or most of the targeted DMMP impurities from spiked PWB.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Surface sampling concentration and reaction probe

A method of analyzing a chemical composition of a specimen is described. The method can include providing a probe comprising an outer capillary tube and an inner capillary tube disposed co-axially within the outer capillary tube, where the inner and outer capillary tubes define a solvent capillary and a sampling capillary in fluid communication with one another at a distal end of the probe; contacting a target site on a surface of a specimen with a solvent in fluid communication with the probe; maintaining a plug volume proximate a solvent-specimen interface, wherein the plug volume is in fluid communication with the probe; draining plug sampling fluid from the plug volume through the sampling capillary; and analyzing a chemical composition of the plug sampling fluid with an analytical instrument. A system for performing the method is also described.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Surface sampling concentration and reaction probe with controller to adjust sampling position

A method of analyzing a chemical composition of a specimen is described. The method can include providing a probe comprising an outer capillary tube and an inner capillary tube disposed co-axially within the outer capillary tube, where the inner and outer capillary tubes define a solvent capillary and a sampling capillary in fluid communication with one another at a distal end of the probe; contacting a target site on a surface of a specimen with a solvent in fluid communication with the probe; maintaining a plug volume proximate a solvent-specimen interface, wherein the plug volume is in fluid communication with the probe; draining plug sampling fluid from the plug volume through the sampling capillary; and analyzing a chemical composition of the plug sampling fluid with an analytical instrument. A system for performing the method is also described.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗