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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 523 records · Page 29
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Microfluidic-Based Robotic Sampling System for Radioactive Solutions

A novel microfluidic based robotic sampling system has been developed for sampling and analysis of liquid solutions in nuclear processes. This system couples the use of a microfluidic sample chip with a robotic system designed to allow remote, automated sampling of process solutions in-cell and facilitates direct coupling of the microfluidic sample chip with analytical instrumentation. This system provides the capability for near real time analysis, reduces analytical waste, and minimizes the potential for personnel exposure associated with traditional sampling methods. A prototype sampling system was designed, built and tested. System testing demonstrated operability of the microfluidic based sample system and identified system modifications to optimize performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Towards a Robust Sampling Approach: A Computational Review and Design

As pointed out in several other works, the estimation of the reliability of the electrical grid can not be conducted without the estimation of the stochastic phenomena of electicity demand and electricity production by variable renewable sources. Therefore, sampling procedures have become integral in the design of engineering structures and analysis. Commonly referred to as Monte Carlo uncertainty analysis or integration, the general objective of these procedures is to establish specifics about the uncertainty of an output characteristic of such an engineering system, given uncertainty about its input characteristics. These sampling procedures are applied in a context in which establishing such specifics cannot be performed through other means. Variance-reduction techniques are designed to lessen the variability among estimators to estimate statistics of those output uncertainties. Importance-sampling techniques, on the other hand, are designed to reduce the number of samples needed to estimate a particular statistic—e.g., a tail probability. The combination of these approaches can reduce the computational burden considerably for a particular estimator and statistic. Importance sampling—geared and designed as it is toward improving a particular estimator—suffers, unfortunately, from the unintended consequence of reducing the performance of other estimators in terms of their variance. The objective of this paper is to offer an alternative sampling procedure where this variance does not grow unacceptably large for a suite of estimators. Moreover, it is anticipated that, with additional knowledge of how an engineering output characteristic responds to its input characteristics, tuning parameters of the input’s sampling procedure can be set to improve the output characteristic’s estimation. This work proves the effectiveness of the suggested alternative approach. Such positive outcome will lead to a decrease of the computational burden of performing stochastic optimization of integrated energy systems (e.g., components dispatch, and portfolio composition). In particular, capturing the contribution to the overall system cost of rare and unlikely events and patterns of the electricity demand and production will become less computationally expensive. This is due to the fact that the approach demonstrated here will allow the sampling of those rare occurrences more frequently without misrepresenting their probabilistic impacts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2013

Expediting Groundwater Sampling at Hanford and Making It Safer - 13158

The CH2M HILL Plateau Remediation Company (CHPRC) manages the groundwater monitoring programs at the Department of Energy's 586-square-mile Hanford site in southeastern Washington state. These programs are regulated by the Resource Conservation and Recovery Act (RCRA), the Comprehensive Environmental Response Compensation and Liability Act (CERCLA), and the Atomic Energy Act (AEA). The purpose of monitoring is to track existing groundwater contamination from past practices, as well as other potential contamination that might originate from RCRA treatment, storage, and disposal (TSD) facilities. An integral part of the groundwater-monitoring program involves taking samples of the groundwater and measuring the water levels in wells scattered across the site. Each year, more than 1,500 wells are accessed for a variety of reasons. Historically, the monitoring activities have been very 'people intensive'. Field personnel or 'samplers' have been issued pre-printed forms showing information about the well(s) for a particular sampling evolution. This information is taken from two official electronic databases: the Hanford Well Information System (HWIS) and the Hanford Environmental Information System (HEIS). The samplers traditionally used these hardcopy forms to document the groundwater samples and well water-levels. After recording the entries in the field, the samplers turned the forms in at the end of the day and other personnel posted the collected information. In Automating Groundwater Sampling at Hanford (HNF-38542-FP Revision 0, Presented at Waste Management 2009 Conference, March 1 - March 5, 2009, Phoenix, AZ), we described the methods, tools, and techniques that would be used in automating the activities associated with measuring water levels. The Field Logging and Electronic Data Gathering (FLEDG) application/database that automates collecting the water-level measurement data has now been implemented at Hanford. In addition to eliminating the need to print out documents, the system saves three-to-four man days each month for the field personnel taking the measurements and the scientists and administrators managing the data and the documentation. After the information has received technical review, FLEDG automatically updates the database for water-level measurements and loads the document management system with the completed sampling report. Due to safety considerations, access to wells is conditional. A spreadsheet with appropriate data not only lists the wells that are cleared for work, but also the safety personnel who must be present before work can start. This spreadsheet is used in planning daily activities. Daily plans are structured to ensure that the wells to be sampled are cleared for work and the appropriate safety personnel have been assigned and are present before the work starts. Historically, the spreadsheets have been prepared manually, and as a result, are potentially subject to human error. However, a companion database application has been developed to work with FLEDG - making the entire sampling process more efficient and safer for personnel. The Well Access List - Electronic, WAL-E, is a database that contains much the same information that was previously manually loaded into the spread sheet. In addition, WAL-E contains a managed work-flow application that shows the access requirements and allows for appropriate reviews of the compiled well. Various CHPRC organizations, including Industrial Hygiene, RADCON, and Well Maintenance and Sample Administration are able to enter and review the wells added or deleted from the WAL-E database. The FLEDG system then accesses this database information to identify appropriate support personnel and provide safety requirements to field personnel. In addition, WAL-E offers the assurance that wells have appropriate locks and are correctly labeled and electrically grounded as required, before well activities begin. This feature is an extremely important aspect of the FLEDG/WAL-E system because it adds another safety check to the work evolution and reduces the potential for unsafe conditions to exist that would lead to a stop-work situation. This paper will further describe the technical aspects of both electronic programs/databases and their successful application at Hanford. (authors)

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Delayed-Gamma Energy Biasing with Exact Energy Sampling in MCNP 6.2.0

Characterization of delayed-particle signatures is of the utmost importance for detecting, identifying, and quantifying special nuclear material (SNM). Various non-destructive assay (NDA) techniques used in nuclear material safeguards rely on characteristic gamma-ray or neutron emissions to infer properties of a material. The all-particle, all-energy Monte-Carlo radiation transport code MCNP6 is capable of simulating delayed-particle signatures from SNM in addition to modeling the transport of emitted particles to a detector or other instrument. In some cases, NDA techniques require the measurement of low probability emissions from a given material. In physical scenarios, this problem can be bypassed by longer count-times or may be simply irrelevant due to the mass, and therefore the total activity, of the material being measured. However, when applying the Monte-Carlo method to such scenarios, sampling of low probability emissions requires a large number of histories to converge to a statistically acceptable solution. To address this issue, the delayed-neutron and gamma energy biasing feature was introduced in MCNP6 by H. Armstrong et al. in 2013 which allows the user to set up energy windows in which delayed-particle emission sampling can be adjusted. For delayed-gamma sampling, this biasing method was based on the bin-wise structure of gamma emission data for both the multi-bin gamma and line-emission sampling modes. Recent improvements have been made to the line-emission sampling algorithm which upgrade the previous mini-bin sampling treatment to an exact energy-line treatment. This upgrade was not compatible with the biasing method implemented by H. Armstrong et al. due to the sampled data no longer having a bin-wise structure in line-emission mode. For this reason the delayed-gamma energy biasing feature has been rewritten to support the exact line-sampling treatment. This paper provides a description of the delayed-gamma energy biasing (DGEB) feature in MCNP6 as well as results and discussion for a gamma-ray spectroscopy example used to demonstrate the biasing utility. (authors)

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Evaluating Manual Sampling Locations for Regulatory and Emergency Response

Drinking water systems commonly use manual or grab sampling to monitor water quality, identify or confirm issues, and verify that corrective or emergency response actions have been effective. In this paper, the effectiveness of regulatory sampling locations for emergency response is explored. An optimization formulation based on the literature was used to identify manual sampling locations to maximize overall nodal coverage of the system. Results showed that sampling locations could be effective in confirming incidents for which they were not designed. When evaluating sampling locations optimized for emergency response against regulatory scenarios, the average performance was reduced by 3%–4%, while using optimized regulatory sampling locations for emergency response reduced performance by 7%–10%. Secondary constraints were also included in the formulation to ensure geographical and water age diversity with minimal impact on the performance. This work highlighted that regulatory sampling locations provide value in responding to an emergency for these networks.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Internet of Samples

Abstract Material samples are indispensable data sources in many natural science, social science, and humanity disciplines. More and more researchers recognize that samples collected in one discipline can be of great value for another. This has motivated organizations that manage a large number of samples to make their holdings accessible to the world. Currently, multiple projects are working to connect natural history and other samples managed by individual institutions or individuals into a universe of samples that follow FAIR principles. This poster reports the progress of the US NSF‐funded iSamples project, in the context of other efforts initiated by US DOE, DiSCCo, BCoN, and GBIF. By October 2021, we will also be able to present an iSamples prototype. We encourage individual organizations that hold material samples to get to know these projects and help shape these projects to realize the goal of a global linked sample cloud that connects all material samples and is accessible to all.

Richard, Stephen M.↗
DOE OSTI2018

Role of Ti Content on the Occurrence of the 3309-cm{sup –1} Peak in FTIR Absorption Spectra of Ruby Samples

The study is based on the determination of trace elements in ruby samples, Ti in particular, using laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS). The samples were then divided into three groups: high (≥ 200 ppma), moderate (100–200 ppma), and low (≤ 50 ppma) Ti content. In addition, X-ray absorption spectroscopy (XAS) was employed to confirm that the Ti oxidation state was Ti{sup 4+}. The heat experiment conditions were set at 800, 1200, and 1650°C to investigate the transformation of the –OH vibration in the FTIR spectra of ruby samples. The FTIR spectra showed that samples containing a low Ti concentration did not show the 3309-cm{sup –1} absorption peak either before or after heating at any of the designed temperatures. An obvious 3309-cm{sup –1} peak appeared only in samples with a moderate to high Ti content after heating at ≥ 1200°C. The results also suggest that, in addition of Ti{sup 4+}, the occurrence of the 3309-cm{sup –1} peak in the FTIR spectra is strongly affected by the charge compensation of –OH in Al sites, i.e., the structural –OH; thus, the structural –Ti–OH stretching in the ruby samples. Hence, for gemological identification, the 3309-cm{sup –1} peak can be applied to indicate whether a ruby has undergone heat treatment if those samples contain enough Ti ions in their structure, i.e., Ti ≥ 100 ppma. This condition is usually found in ruby samples from major deposits such as Mong Hsu and Mogok, Myanmar; Luc Yen, Vietnam; and Montopuez, Mozambique.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Production Procedure and Characterization of Zn-Doped Y-123 Superconducting Samples Prepared by Sol-Gel Method

The superconducting YBa{sub 2}Cu{sub 3−x}Zn{sub x}O{sub 7} (Y-123) bulk materials have been synthesized by using the sol-gel method. Samples are produced as undoped Y-123 and transition metal (Zn)-doped Y-123. Before the final heat treatment, the samples are calcined at 850 °C for 24 h. This process is repeated three times. Then, samples are sintered at 950 °C for 24 h in an air environment and at 500 °C for 5 h in an oxygen atmosphere. The synthesized products are characterized by XRD, R-T, and Vickers microhardness tester. The XRD investigation revealed that the prepared sample has an orthorhombic structure. According to XRD measurements, an orthorhombic structure has not changed with Zn doping. It was observed that undoped and Zn-doped samples have superconductivity properties by electrical measurements. T{sub c}{sup onset} is 89 K for undoped Y-123 sample, and the T{sub c}{sup onset} value decreases monotically with Zn addition. All samples show metallic behavior above T{sub c}{sup onset} temperature. As a result of Vickers microhardness measurements, it is observed that all samples have reverse indentation size effect (RISE) behavior.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Rapid determination of radiostrontium in seawater samples

A new method for the determination of radiostrontium in seawater samples has been developed at the Savannah River National Laboratory (SRNL) that allows rapid preconcentration and separation of strontium and yttrium isotopes in seawater samples for measurement. The new SRNL method employs a novel and effective pre-concentration step that utilizes a blend of calcium phosphate with iron hydroxide to collect both strontium and yttrium rapidly from the seawater matrix with enhanced chemical yields. The pre-concentration steps, in combination with rapid Sr Resin and DGA Resin cartridge separation options using vacuum box technology, allow seawater samples up to 10 liters to be analyzed. The total 89 Sr + 90 Sr activity may be determined by gas flow proportional counting and recounted after ingrowth of 90 Y to differentiate 89 Sr from 90 Sr. Gas flow proportional counting provides a lower method detection limit than liquid scintillation or Cerenkov counting and allows simultaneous counting of samples. Simultaneous counting allows for longer count times and lower method detection limits without handling very large aliquots of seawater. Seawater samples up to 6 liters may be analyzed using Sr Resin for 89 Sr and 90 Sr with a Minimum Detectable Activity (MDA) of 1-10 mBq/L, depending on count times. Seawater samples up to 10 liters may be analyzed for 90 Sr using a DGA Resin method via collection and purification of 90 Y only. If 89 Sr and other fission products are present, then 91 Y (beta energy 1.55 MeV, 58.5 day half-life) is also likely to be present. 91 Y interferes with attempts to collect 90 Y directly from the seawater sample without initial purification of Sr isotopes first and 90 Y ingrowth. The DGA Resin option can be used to determine 90 Sr, and if 91 Y is also present, an ingrowth option with using DGA Resin again to collect 90 Y can be performed. An MDA for 90 Sr of <1 mBq/L for an 8 hour count may be obtained using 10 liter seawater sample aliquots.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2018

Efficient Surrogate Model Development: Impact of Sample Size and Underlying Model Dimensions

This study compares eight surrogate-model construction approaches using computational experiments. Here, the construction approaches considered include: Artificial Neural Networks (ANNs), Automated Learning of Algebraic Models using Optimization (ALAMO), Radial Basis Networks (RBNs), Extreme Learning Machines (ELMs), Gaussian Progress Regression (GPR), Random Forests (RFs), Support Vector Regression (SVR), and Multivariate Adaptive Regression Splines. Each approach is used to construct surrogate models for predicting the outputs of thirty-four test functions. The data used to construct surrogate models were generated using Latin Hypercube Sampling (LHS), Halton and Sobol sampling methods. We studied the impact of sampling method, sample size, and challenge function characteristics on the accuracy of surrogate model predictions. Our results revealed that for smaller sample sizes, on average, surrogate models trained using the data points generated by Sobol sequences provided the best estimation for all surrogate model construction approaches. As the sample size increased, the impact of sampling methods diminished. The comparison of surrogate-modeling construction approaches at large sample sizes revealed that surrogate models trained using ANN, ALAMO, and ELM yielded smaller root mean squared error and higher adjusted R-squared values than the models trained using the rest of the approaches.

42 ENGINEERING↗
DOE OSTI2025

Comparison of measurement techniques and sorption of radium-226 in low and high salinity aqueous samples

Human activities have the potential to redistribute radium (Ra) in the marine environment in a manner that may necessitate monitoring or management of subsequent human or environmental exposures. There is therefore a need to identify accurate and accessible techniques for Ra measurement in high salinity samples and to describe the distribution of Ra in estuarine and marine environments, but most efforts in these areas have focused on low salinity matrices. In addition, rapid and reliable measurements are crucial for time-sensitive samples such as short-lived isotopes or emergency situations. The objective of this study is to describe the limits of detection, cost, and relative ease for measurement of Ra in both low and high salinity aqueous samples via three analytical methods: liquid scintillation counting (LSC), high purity germanium (HPGe) gamma spectrometry, and inductively coupled plasma mass spectrometry (ICP-MS). To contextualize these measurements for real-world scenarios, the partitioning of 226 Ra to substrates relevant to the marine environment was also characterized. Although HPGe detection with solid phase extraction had the lowest limit of detection for low salinity samples (0.27 Bq L −1 ), poor 226 Ra recovery for high salinity samples and high materials costs make this method prohibitive for many users. Limits of detection for high salinity samples were lower for LSC (1.28 Bq L −1 ) than for ICP-MS without dilution (11.4 Bq L −1 ), but significant and unexpected degradation of the high salinity LSC standards was observed after six months. Furthermore, our preferred measurement method for high salinity Ra samples is ICP-MS with sample dilution as necessary to reduce matrix effects.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2021

Sample environment effects on synchrotron-measured temperature profiles in an approximant of optical floating zone crystal growth

Even though the growth of crystals using optical floating zone furnaces has had an immense scientific impact, the implementation of this method remains more of an art than a science due to the difficulty of obtaining quantitative information about the sample thermal profile during crystal growth. Building on recent work demonstrating that in situ synchrotron studies can be used to map sample rod temperatures during heating, investigations were carried out to better understand how the sample environment affects the sample temperature profile. Through a combination of experimental studies and modeling efforts, it is shown that the environment in the furnace can strongly influence the sample temperature at the lamp focus, the steepness of the vertical temperature gradient, and the timescale required for sample heating and cooling - effects which can combine to produce a strong history-dependence to sample temperature profiles. It is demonstrated that the furnace effects can be effectively captured in thermal models, allowing both the steady-state and time-dependent behavior of the sample to be accurately reproduced with predictive models, and providing a launching point for improved furnace designs that can more readily deliver desired thermal profiles.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Automated Coupling of Nanodroplet Sample Preparation with Liquid Chromatography–Mass Spectrometry for High-Throughput Single-Cell Proteomics

Single-cell proteomics can provide critical biological insight into the cellular heterogeneity that is masked by bulk-scale analysis. Here, we have developed a nanoPOTS (nanodroplet processing in one pot for trace samples) platform and demonstrated its broad applicability for single-cell proteomics. However, because of nanoliter-scale sample volumes, the nanoPOTS platform is not compatible with automated LC-MS systems, which significantly limits sample throughput and robustness. To address this challenge, we have developed a nanoPOTS autosampler allowing fully automated sample injection from nanowells to LC-MS systems. We also developed a sample drying, extraction, and loading workflow to enable reproducible and reliable sample injection. The sequential analysis of 20 samples containing 10 ng tryptic peptides demonstrated high reproducibility with correlation coefficients of >0.995 between any two samples. The nanoPOTS autosampler can provide analysis throughput of 9.6, 16, and 24 single cells per day using 120, 60, and 30 min LC gradients, respectively. As a demonstration for single-cell proteomics, the autosampler was first applied to profiling protein expression in single MCF10A cells using a label-free approach. At a throughput of 24 single cells per day, an average of 256 proteins was identified from each cell and the number was increased to 731 when the Match Between Runs algorithm of MaxQuant was used. Using a multiplexed isobaric labeling approach (TMT-11plex), ~77 single cells could be analyzed per day. We analyzed 152 cells from three acute myeloid leukemia cell lines, resulting in a total of 2558 identified proteins with 1465 proteins quantifiable (70% valid values) across the 152 cells. These data showed quantitative single-cell proteomics can cluster cells to distinct groups and reveal functionally distinct differences.

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

Femtosecond Laser Desorption Postionization MS vs ToF-SIMS Imaging for Uncovering Biomarkers Buried in Geological Samples

The study of lipid molecular fossils by traditional biomarker analysis requires bulk sample crushing, followed by solvent extraction, and then the analysis of the extract by gas chromatography-mass spectrometry (GC–MS). This traditional analysis mixes all organic compounds in the sample regardless of their origins, with a loss of information on the spatial distribution of organic molecules within the sample. These shortcomings can be overcome using the chemical mapping of intact samples. Spectroscopic techniques such as UV fluorescence or Raman spectroscopy, laser ablation inductively coupled plasma mass spectrometry, and time-of-flight secondary ion mass spectrometry (ToF-SIMS) are among those elemental and molecular mapping techniques. This study employed femtosecond (fs) laser ablation combined with single-photon ionization, a method called fs-laser desorption postionization mass spectrometry (fs-LDPI-MS). In this work, a pulsed ~75 fs, 800 nm laser was used to ablate the geological sample, which was then photoionized after a few microseconds by a pulsed 7.9 eV vacuum ultraviolet laser. An organic carbon-rich geological sample was used for this study to map hydrocarbon biomarkers in sediments that were previously studied by GC–MS. The petrography of this sample was examined by optical and fluorescence microscopy. It is demonstrated here that fs-LDPI-MS combined with petrography for multimodal imaging can expose buried compounds within the sample via in situ layer removal. When used in conjunction with traditional organic geochemical analysis, this method has the potential to determine the spatial distribution of organic biomarkers in geological material. Finally, fs-LDPI-MS imaging data are compared with ToF-SIMS imaging that is commonly used for such studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Block Design with Common Reference Samples Enables Robust Large-Scale Label-Free Quantitative Proteome Profiling

Label-free quantitative proteomics has become an increasingly popular tool for profiling global protein abundances. However, one major weakness is the potential performance drift of the LC-MS platform over time, which in turn limits its utility for analyzing large-scale sample sets. To address this, in this work we introduce an experimental and data analysis scheme based on a block-design with common controls within each block for enabling LC-MS-based large-scale label-free quantification. In this scheme, a large number of samples (e.g., >100 samples) are analyzed in smaller, and more manageable blocks, minimizing instrument drift and variability within a block. Furthermore, each designated block also contains common controls (or reference) samples for normalization within and across blocks. We demonstrated the effectiveness of this method by profiling the proteome response of human macrophage THP-1 cells to 11 engineered nanomaterials (ENMs) at two different doses. A total of 116 samples were analyzed in six blocks, yielding an average coverage of 4500 proteins per sample. The data revealed consistent quantification of proteins across all six blocks, as shown by highly stable quantification of house-keeping proteins in all samples and high levels of quantification correlation among samples from different blocks. The data also demonstrated that label-free quantification is robust and accurate enough to quantify even very subtle abundance changes as well as large fold-changes without potential ratio compression as often encountered with isobaric labeling. Our streamlined workflow is easy to implement and can be readily adapted to other large cohort studies for reproducible label-free proteome quantification.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2015

Nanopipettes: probes for local sample analysis

Nanopipettes (pipettes with diameters <1 μm) were explored as pressure-driven fluid manipulation tools for sampling nanoliter volumes of fluids. The fundamental behavior of fluids confined in the narrow channels of the nanopipette shank was studied to optimize sampling volume and probe geometry. This method was utilized to collect nanoliter volumes (<10 nL) of sample from single Allium cepa cells and live Drosophila melanogaster first instar larvae. Matrix assisted laser desorption/ionization-mass spectrometry (MALDI-MS) was utilized to characterize the collected sample. The use of nanopipettes for surface sampling of mouse brain tissue sections was also explored. Lipid analyses were performed on mouse brain tissues with spatial resolution of sampling as small as 50 μm. Nanopipettes were shown to be a versatile tool that will find further application in studies of sample heterogeneity and population analysis for a wide range of samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Direct and rapid uranium isotopic analysis of environmental sample swipes via microextraction – LS-APGD/Orbitrap mass spectrometry

Accurate and precise isotopic analysis of actinides collected on environmental sample swipes from within nuclear facilities is an important safeguarding measure for detecting undeclared materials and activities. Traditional isotope ratio (IR) analysis of actinides using a bulk digestion approach can be laborious and time-consuming. Recently, direct analysis of environmental swipe samples using a microextraction approach has been explored as an alternative to conventional bulk digestion methods. The present study further evaluates this approach for accurate and precise isotopic analysis of uranium (U) in cotton swipe samples using the liquid sampling-atmospheric pressure glow discharge (LS-APGD)/Orbitrap-FTMS Booster detection system. The instrumental parameters were optimized, and quantitative capabilities were demonstrated through excellent linearity (R2 = 0.99) across a deposited mass range of 1 to 500 ng, with a limit of detection of 90 pg (in a 2 × 4 mm region) for total U; well below typical U concentrations (ng–mg range) in environmental sample swipes. The 235U/238U ratio showed excellent accuracy (−0.3% relative difference from the certificate value), with ∼20× improvement over previous microextraction-Orbitrap methods. Precision (∼1% relative standard deviation) was also greatly enhanced by ∼5×. This study also demonstrates that figures of merit achieved with neat U solution were not highly degraded when various external interfering elements/matrices were introduced. Finally, the developed method was successfully applied to analyze practical swipe samples representative of laboratory and outdoor environments. The presented figures of merit and applicability to practical samples further validate the capability of the platform for rapid analysis (<7 minutes) of environmental swipe samples.

Shrestha, Suraj [Clemson University, SC]↗
DOE OSTI2013

Qualitative analysis of Pb liquid sample using laser-induced breakdown spectroscopy (LIBS)

Qualitative analysis of liquid sample containing 1,000 ppm of Pb was performed by using LIBS technique. In order to avoid splashing off of the liquid sample during laser irradiation, a sample pretreatment was done, namely the liquid sample was absorbed by using commercial available stomach medicine. Two kinds of absorbent materials were chosen in this experiment, first containing 125 mg activated carbon and second 600 mg activated attapulgite. These absorbent materials were used since carbon sample gives better absorption of infrared laser irradiation used in this experiment. In order to characterize the absorption process, three treatments were conducted in this experiment; first, without heating the sample but varying the absorption time before laser irradiation; second by varying the heating temperature after certain time of absorption process and third by varying the temperature only. The maximum emission intensity of Pb I 405.7 nm was found in the second treatment of heating the sample till 85°C after 30 minutes absorption of the liquid sample in both absorbent materials.

36 MATERIALS SCIENCE↗