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DOE OSTI2019

Single-Grain Bulk YBa{sub 2}Cu{sub 3}O{sub y} Superconductor Grown in Shorter Duration by IG Process

The top-seeded infiltration growth (IG) process is considered to be an attractive, well-established route compared to melt growth (MG) process due to its successful ability to resolve observed problems in MG process such as pores, shrinkage, and an ununiformed Y{sub 2}BaCuO{sub 5} (Y-211) secondary phase particle dispersion in Y-123 matrix. This is among the first accounts of superconductivity where a large grain YBa{sub 2}Cu{sub 3}O{sub y} (Y-123) was produced by IG process. Further, by utilizing homemade Y-123 and Y-211, we had prepared YBa{sub 2}Cu{sub 3}O{sub y} samples via Y-123 + liquid (1:1) as a liquid source and had further characterized by utilizing the scanning electron microscopy (SEM), superconducting transition temperature (T{sub c}), and critical current density (J{sub c}) at 77 K. Here, we provide temperature dependence of magnetization measurements that indicated a sharp superconducting transition with T{sub c} (onset) around 92 K. In addition, the critical current density was calculated on the basis of Bean’s model and resulted as 30,000 A/cm{sup 2} at 77 K (self-field), H//c-axis. Trapped field experiments had lucidly indicated that single-grain nature with maximum-trapped field of 0.3 T at 77 K and 1 mm above sample surface even samples are produced shorter duration, i.e., 50 h.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2017

Investigation and Applications of In-Source Oxidation in Liquid Sampling-Atmospheric Pressure Afterglow Microplasma Ionization (LS-APAG) Source

A liquid sampling-atmospheric pressure afterglow microplasma ionization (LS-APAG) source is presented for the first time, which is embedded with both electrospray ionization (ESI) and atmospheric pressure afterglow microplasma ionization (APAG) techniques. This ion source is capable of analyzing compounds with diverse molecule weights and polarities. An unseparated mixture sample was detected as a proof-of-concept, giving complementary information (both polarities and non-polarities) with the two ionization modes. It should also be noted that molecular mass can be quickly identified by ESI with clean and simple spectra, while the structure can be directly studied using APAG with in-source oxidation. The ionization/oxidation mechanism and applications of the LS-APAG source have been further explored in the analysis of nonpolar alkanes and unsaturated fatty acids/esters. A unique [M + O – 3H]{sup +} was observed in the case of individual alkanes (C{sub 5}–C{sub 19}) and complex hydrocarbons mixture under optimized conditions. Moreover, branched alkanes generated significant in-source fragments, which could be further applied to the discrimination of isomeric alkanes. The technique also facilitates facile determination of double bond positions in unsaturated fatty acids/esters due to diagnostic fragments (the acid/ester-containing aldehyde and acid oxidation products) generated by on-line ozonolysis in APAG mode. Finally, some examples of in situ APAG analysis by gas sampling and surface sampling were given as well. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2015

Results of Hg Speciation Testing on Tank 38 and 2H Evaporator Overhead Tank (OHT-1) Materials

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The seventh shipment of samples was designated to include two Tank 38 (2H Evaporator System Drop Tank) samples: a surface sample (HTF-38-15-48) and a variable depth sample taken at 265” (HTF-38-15-50). The third sample submitted was from the 2H Evaporator Overhead Tank (OHT) #1. All samples were received by SRNL on May 11, 2015. The OHT-1 was not placed in the SRNL Shielded Cells but was instead placed in a refrigerator in 773-A, B-wing upon receipt and kept at 4°C. The Tank 38 samples were left in their stainless steel dip bottles until they were opened and an aliquot of each diluted 1:10 with Eurofins deionized water on June 1, 2015. Following initial dilution in the Shielded Cells, the diluted Tank 38 samples were immediately moved to refrigeration and kept in the dark until prepared for shipment to Eurofins.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2015

Results of HG Speciation Testing on Tank 43 and 2H Evaporator Overhead Tank (OHT-2) Materials

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The eighth shipment of samples was designated to include two Tank 43 (2H Evaporator System Feed Tank) samples: a surface sample (HTF-43-15-52) and a variable depth sample taken at 161” (HTF-43-15-54). The third sample submitted was from the 2H Evaporator Overhead Tank (OHT) #2. All samples were received by SRNL on May 11, 2015. The OHT-2 was not placed in the SRNL Shielded Cells but was instead placed in a refrigerator in 773-A, B-wing upon receipt and kept at 4°C. The Tank 43 samples were left in their stainless steel dip bottles until they were opened and an aliquot of each diluted 1:10 with Eurofins deionized water on June 3, 2015. Following initial dilution in the Shielded Cells, the diluted Tank 43 samples were immediately moved to refrigeration and kept in the dark until prepared for shipment to Eurofins.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1974

Apparatus for microbiological sampling

An automatic apparatus is described for microbiologically sampling surface using a cotton swab which eliminates human error. The apparatus includes a self-powered transport device, such as a motor-driven wheeled cart, which mounts a swabbing motor drive for a crank arm which supports a swab in the free end thereof. The swabbing motor is pivotably mounted and an actuator rod movable responsive to the cart traveling a predetermined distance provides lifting of the swab from the surface being sampled and reversal of the direction of travel of the cart.

Wilkins, J. R.↗

DOE OSTI2021

High efficiency environmental sampling with rapidly cured peelable coatings

A rapidly curable liquid gel for collecting an analyte from a sampling surface includes a polymer precursor mixture including a monomer and/or an oligomer; and an additive to enhance extraction of the analyte from the sampling surface. A kit for collecting an analyte from a sampling surface may include the rapidly curable liquid gel and a portable device for rapidly curing the gel. The rapidly curable liquid gel is cured to thereby form a peelable sampling film, and the sampling film is removed from the sampling surface, thereby collecting the analyte. In one embodiment, the rapidly curable liquid gel is UV-curable, the polymer precursor mixture further includes a photoinitiator compound, and the portable device includes a UV light source configured to emit UV light of a wavelength range absorbed by the photoinitiator compound.

Henzl, Vladimir↗

DOE OSTI2018

Analysis of Tank 30H (HTF-30-18-54, -55), Tank 32H (HTF-32-18-56, -57), and Tank 37H (HTF-37-18-58, -59) Samples for Support of the Evaporator Feed Qualification and Corrosion Control Programs for the 3H-Evaporator

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2011

Summary of Surface Swipe Sampling for Beryllium on Lead Bricks and Shielding

Approximately 25,000 lbs of lead bricks at Site 300 were assessed by the Site 300 Industrial Hygienis tand Health Physicist for potential contamination of beryllium and radiation for reuse. These lead bricks and shielding had been used as shielding material during explosives tests that included beryllium and depleted uranium. Based on surface swipe sampling that was performed between July 26 and October 11, 2010, specifically for beryllium, the use of a spray encapsulant was found to be an effective means to limit removable surface contamination to levels below the DOE release limit for beryllium, which is 0.2 mcg/100 cm{sup 2}. All the surface swipe sampling data for beryllium and a timeline of when the samples were collected (and a brief description) are presented in this report. On December 15, 2010, the lead bricks and shielding were surveyed with an ion chamber and indicated dose rates less than 0.05 mrem per hour on contact. This represents a dose rate consistent with natural background. An additional suevey was performed on February 8, 2011, using a GM survey instrument to estimate total activity on the lead bricks and shielding, confirming safe levels of radioactivity. The vendor is licensed to possess and work with radioactive material.

61 RADIATION PROTECTION AND DOSIMETRY↗

DOE OSTI2011

Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESA mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.

Direct liquid extraction↗

DOE OSTI2019

Analysis of Tank 30H (HTF-30-19-33, -34), Tank 32H (HTF-32-19-35, -36), and Tank 37H (HTF-37-19-53, -54) Samples for Support of the Evaporator Feed Qualification and Corrosion Control Programs for the 3H-Evaporator

SRNL analyzed samples from Tank 30H, Tank 32H, and Tank 37H to support the Evaporator Feed Qualification and Corrosion Control Programs for the 3H-Evaporator system. The six samples from Tanks 30H, 32H, and 37H all contain highly concentrated salt solutions with sodium concentrations ranging from 13.8 M to 16.9 M. Hydroxide is the dominant anion in all of the samples followed by nitrate and nitrite. The preponderance of the analytical determinations (density, anions, cations) on all three tanks show slightly higher concentrations of solute in the sub-surface sample than in the surface sample, indicating some stratification within the tanks. With the exception of the Tank 30H VDS, all of the samples are somewhat more concentrated compared with the compositions of the previous samples. The sum of the major cations versus the sum of the major anions show a difference of <5% for all of the samples indicating good data quality for the non-radioactive analytes in the table. The silicon concentrations measured in the VDS and surface samples from Tank 30H, Tank 32H, and Tank 37H were all below detection.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Analysis of Tank 30H (HTF-30-19-33, -34), Tank 32H (HTF-32-19-35, -36), and Tank 37H (HTF-37- 19-53, -54) Samples for Support of the Evaporator Feed Qualification and Corrosion Control Programs for the 3H-Evaporator

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Mechanisms of dissolution from gibbsite step edges elucidated by ab initio molecular dynamics with enhanced sampling

Surface reactions underpin our collective understanding of mineral dissolution. This impacts a range of predictive geochemical models (for weathering, the fate and transport of metals) as well as industrial utilization of minerals. Yet atomistic details are rarely known due to the complex mineral/fluid interfacial environment. There is significant need to understand the mechanistic details of dissolution reactions and how they depend on surface morphology and solution conditions. This work utilizes surface pit models in conjunction with changes to solution composition that mimic pH to explore surface detachment of aluminate from gibbsite, which is a primary source of Al in soils and within the industrial processing of aluminum. Ab initio molecular dynamics simulations with enhanced sampling has been used to explore the detailed process of the detachment, the results of which indicate two potential pathways that are differentiated based upon the extent of water hydration. Here, the heights of the energy barriers depend upon the local morphology which influence the number of bridges (quasi-)simultaneously broken (1 or 2) or the Al-O coordination of the neighboring aluminum atoms (5 or 6) at the armchair edge. pH effects are significant, with a nearly 50% reduction in barrier height under alkaline conditions that are relevant to geothermal fluids and Al extraction from minerals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Data Validation Package November 2015 Groundwater and Surface Water Sampling at the Old and New Rifle, Colorado, Processing Sites February 2016

Water samples were collected from 36 locations at New Rifle and Old Rifle, Colorado, Processing Sites. Duplicate samples were collected from New Rifle locations 0659 and 0855, and Old Rifle location 0304. One equipment blank was collected after decontamination of non-dedicated equipment used to collect one surface water sample. Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). New Rifle Site Samples were collected at the New Rifle site from 16 monitoring wells and 7 surface locations in compliance with the December 2008 Groundwater Compliance Action Plan [GCAP] for the New Rifle, Colorado, Processing Site (LMS/RFN/S01920), with one exception: New Rifle location 0635 could not be sampled because it was inaccessible; a fence installed by the Colorado Department of Transportation prevents access to this location. DOE is currently negotiating access with the Colorado Department of Transportation. Analytes measured at the New Rifle site included contaminants of concern (COCs) (arsenic, molybdenum, nitrate + nitrite as nitrogen, selenium, uranium, and vanadium) ammonia as nitrogen, major cations, and major anions. Field measurements of total alkalinity, oxidation- reduction potential, pH, specific conductance, turbidity, and temperature were made at each location, and the water level was measured at each sampled well. A proposed alternate concentration limit (ACL) for vanadium of 50 milligrams per liter (mg/L), specific to the compliance (POC) wells (RFN-0217, -0659, -0664, and -0669) is included in the New Rifle GCAP. Vanadium concentrations in the POC wells were below the proposed ACL as shown in the time-concentration graphs in the Data Presentation section (Attachment 2). Time-concentration graphs from all other locations sampled are also included in Attachment 2. Sampling location RFN-0195 was misidentified for the June/August 2014 and November 2014 sampling events. (Well RFN-0609 was inadvertently sampled instead of RFN-0195 in 2014.) The results for RFN-0195 have been corrected, and are included in associated time-concentration graphs for this location. Recent results for RFN-0195 are consistent with established trends with the possible exception of vanadium. The most recent result for vanadium showed an increase over recent values. Vanadium concentrations at RFN-0195 and other locations will continue to be evaluated in the future to determine the potential for deviations from established trends. The surface water locations were sampled to monitor the impact of groundwater discharge. COC concentrations at Colorado River surface water locations RFN-0324 and RFN-0326, downgradient of the site, remained low and were consistent with historical results, as shown in the time-concentration graphs. COC concentrations did not indicate there are any impacts related to groundwater discharge to the river. In many cases, elevated COC concentrations at the New Rifle site pond locations were observed, as shown in the time-versus concentration graphs. As noted in the GCAP, this indicates impacts from groundwater discharge to the ponds. Old Rifle Site Samples were collected at the Old Rifle site from eight monitoring wells and five surface locations in compliance with the December 2001 Groundwater Compliance Action Plan for the Old Rifle, Colorado, UMTRA Project Site (GJ0-2000-177-TAR). Analytes measured at the Old Rifle site included COCs (selenium, uranium, and vanadium), major cations, and major anions. Field measurements of total alkalinity, oxidation-reduction potential, pH, specific conductance, turbidity, temperature, were made at each location, and the water level was measured at each sampled well. The monitoring strategy described in the GCAP is designed to determine progress of the natural flushing process in meeting compliance standards for site COCs. Standards for selenium and vanadium are the proposed ACLs of0.05 mg/L and 1.0 mg/L, respectively. For uranium the cleanup goal is the UMTRA standard of 0.044 mg/L or background, whichever is higher. As shown in the time concentration graphs, the uranium concentration exceeds the cleanup goal at groundwater monitoring locations RF0-0304, -0305, -0310, -0655, and -0656. The surface water locations were sampled to monitor the impact of groundwater discharge at Colorado River surface water locations adjacent to (RF0-0396) and downgradient of the site (RF0-0741). COC concentrations remain low and consistent with historical concentrations as shown in the time-concentration graphs (Attachment 2), which indicate no impacts from groundwater discharge to the river.

2015 Old and New Rifle↗

DOE OSTI2016

Data Validation Package June 2016 Groundwater and Surface Water Sampling at the Old and New Rifle, Colorado, Processing Sites September 2016

Sampling Period: June 14–17 and July 7, 2016. Water samples were collected from 36 locations at New Rifle and Old Rifle, Colorado, Disposal/Processing Sites. Planned monitoring locations are shown in Attachment 1, Sampling and Analysis Work Order. Duplicate samples were collected from New Rifle locations 0216 and 0855, and Old Rifle location 0655. One equipment blank was collected after decontamination of non-dedicated equipment used to collect one surface water sample. See Attachment 2, Trip Report for additional details. Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated, http://energy.gov/lm/downloads/sampling-and- analysis-plan-us-department-energy-office-legacy-management-sites). New Rifle Site Samples were collected at the New Rifle site from 16 monitoring wells and 7 surface locations in compliance with the December 2008 Groundwater Compliance Action Plan [GCAP] for the New Rifle, Colorado, Processing Site (LMS/RFN/S01920). Monitoring well 0216 could not be sampled in June because it was surrounded by standing water due to the high river stage from spring runoff, it was later sampled in July. Monitoring well 0635 and surface location 0322 could not be sampled because access through the elk fence along Interstate 70 has not been completed at this time. Old Rifle Site Samples were collected at the Old Rifle site from eight monitoring wells and five surface locations in compliance with the December 2001 Ground Water Compliance Action Plan for the Old Rifle, Colorado, UMTRA Project Site (GJ0-2000-177-TAR).

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

An organogel library for solution NMR analysis of nanoparticle suspensions in non-aqueous samples

Surface contrast solution NMR methods (scNMR) are emerging as powerful tools to investigate the adsorption of small molecule ligands to the surface of nanoparticles (NP), returning fundamental insight into the kinetics and thermodynamics of sorption, as well as structural information on the adsorbed species. A prerequisite for the acquisition of high quality solution NMR data is the preparation of homogeneous and stable samples that return consistent NMR spectra and allow extensive signal averaging. Unfortunately, this condition does not apply to NMR samples containing NPs that often show a tendency to sediment and accumulate at the bottom of the NMR tube over the course of the experiment. We have recently shown that preparing NMR samples in an agarose gel matrix inhibits sedimentation and allows the characterization of small molecule-NP interactions by scNMR. Unfortunately, as the agarose gel only forms in aqueous solution, this sample preparation method cannot be used to stabilize NP suspensions in a non-aqueous environment. In this work, we introduce a library of 48 organogels, based on low molecular-mass organic gelators (LMOGs), to prepare NMR samples of small molecule/NP systems in a wide range of organic solvents. In addition, we present a simple method that takes advantage of 1H transverse relaxation (1H-R2) measurements to screen the library and identify the best gelator to characterize the small molecule-NP interaction of interest in the solvent of choice. We expect the results of this study will enable the preparation of homogeneous and stable samples of NPs in non-aqueous environments, therefore dramatically increasing the applicability of scNMR to the characterization of heterogeneous interactions and to the investigation of the role played by solvent molecules in regulating the kinetics and thermodynamics of sorption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Speedy Acquisition of Surface-Contamination Samples

Biological contamination of large-area surfaces can be determined quickly, inexpensively, and accurately with the aid of a polyester bonded cloth. Cloth is highly effective in removing microbes from a surface and releasing them for biological assay. In releasing contaminants, polyester bonded cloth was found to be superior to other commercial cleanroom cloths, including spun-bound polyamid cloths and cellulose cloths.

Puleo, J. R.↗

DOE OSTI2021

Absolute quantitation of propranolol from 200-μm regions of mouse brain and liver thin tissues using laser ablation-dropletProbe-mass spectrometry

Rationale: The ability to quantify drugs and metabolites in tissue with sub-mm resolution is a challenging but much needed capability in pharmaceutical research. To fill this void, a novel surface sampling approach combining laser ablation with the commercial dropletProbe automated liquid surface sampling system (LA-dropletProbe) was developed and presented here.Methods: Parylene C-coated 200 × 200 μm tissue regions of mouse brain and kidney thin tissue sections were analyzed for propranolol by laser ablation of tissue directly into a preformed liquid junction. Propranolol was detected by high performance liquid chromatography with positive ion mode electrospray ionization tandem mass spectrometry. Quantitation was achieved via application of a stable isotope-labeled internal standard and an external calibration curve.Results: Absolute concentration of propranolol determined from 200 × 200 µm tissue regions were compared to propranolol concentrations obtained from 2.3-mm-diameter tissue punches of adjacent, non-coated sections using standard bulk tissue extraction protocols followed by regular HPLC-MS/MS analysis. Average concentration of propranolol in both organs determined by the two employed methods agreed within ±12%. Furthermore, the relative abundance of phase II hydroxypropranolol glucuronide metabolites were recorded and found to be consistent with previous results.Conclusions: This work illustrates that depositing a thin parylene C layer onto thin tissue prior to analysis, which seals the surface and prevents direct liquid extraction of the drug from the tissue, coupled to the novel LA-dropletProbe surface sampling system is a viable approach for sub-mm resolution quantitative drug distribution analysis.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS1999

3-D Surface Depression Profiling Using High Frequency Focused Air-Coupled Ultrasonic Pulses

Surface topography is an important variable in the performance of many industrial components and is normally measured with diamond-tip profilometry over a small area or using optical scattering methods for larger area measurement. This article shows quantitative surface topography profiles as obtained using only high-frequency focused air-coupled ultrasonic pulses. The profiles were obtained using a profiling system developed by NASA Glenn Research Center and Sonix, Inc (via a formal cooperative agreement). (The air transducers are available as off-the-shelf items from several companies.) The method is simple and reproducible because it relies mainly on knowledge and constancy of the sound velocity through the air. The air transducer is scanned across the surface and sends pulses to the sample surface where they are reflected back from the surface along the same path as the incident wave. Time-of-flight images of the sample surface are acquired and converted to depth/surface profile images using the simple relation (d = V*t/2) between distance (d), time-of-flight (t), and the velocity of sound in air (V). The system has the ability to resolve surface depression variations as small as 25 microns, is useable over a 1.4 mm vertical depth range, and can profile large areas only limited by the scan limits of the particular ultrasonic system. (Best-case depth resolution is 0.25 microns which may be achievable with improved isolation from vibration and air currents.) The method using an optimized configuration is reasonably rapid and has all quantitative analysis facilities on-line including 2-D and 3-D visualization capability, extreme value filtering (for faulty data), and leveling capability. Air-coupled surface profilometry is applicable to plate-like and curved samples. In this article, results are shown for several proof-of-concept samples, plastic samples burned in microgravity on the STS-54 space shuttle mission, and a partially-coated cylindrical ceramic composite sample. Impressive results were obtained for all samples when compared with diamond-tip profiles and measurements from micrometers. The method is completely nondestructive, noninvasive, non-contact and does not require light-reflective surfaces.

Roth, Don J.↗