Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Radiochemical Analysis”

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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
NASA NTRS1984

On the chondrite-achondrite transition - Mineralogy and chemistry of Yamato 74160 (LL7)

Petrology, mineralogic properties and contents of major elements and trace elements Ag, Au, Bi, Cd, Co, Cs, Ga, In, Rb, Se, Te, Tl, U and Zn are reported (determined by radiochemical neutron activation analysis) in Yamato 74160, interpreted as an LL7 chondrite. All properties are consistent with this meteorite having been recrystallized and partially melted locally once at temperatures well above 1090 C under conditions such that some minerals (e.g. plagioclase, euhedral pyroxene, tetrataenite) grew from melt pockets and siderophilic and chalcophilic elements were lost by extraction into eutectic melt that drained away. Inhomogeneous plagioclase compositions and mobile element loss suggest shock as the most likely heat source. Yamato 74160, while inferentially chondritic, is a larval achondrite: even higher temperatures and longer times would have been required to cause the separations necessary to transform it to an identifiable achondrite type.

Takeda, H.↗
NASA NTRS1985

Mobile trace element contents in Jilin chondrite

A determination is conducted of ppm-ppt levels of Co, Se, Ga, Rb, Cs, Te, Bi, Ag, In, Tl, Zn and Cd (arranged empirically in order of increasing mobility at 1000 C) by radiochemical neutron activation analysis in eight Jilin samples of known Ar-40 content and a large vein from one of these. The trace element contents of the vein do not differ markedly from those of Jilin whole-rock samples. Only Rb correlates with Ar-40, possibly due to chance. All elements but Cd are present at levels similar to thdse in H4-6 chondrites with long K/Ar age (i.e., presumably mildly shocked). These levels are low relative to those in analogous L4-6 chondrites suggesting that H chondrites formed and/or evolved under higher pre-shock temperatures than did mildly shocked L chondrites. Time-temperature conditions during shock-loading of Jilin parent material were mild relative to those in strongly shocked L chondrites, being sufficient at most only to mobilize Cd.

Sakuragi, Y.↗
NASA NTRS1985

The origin and history of the metal and sulfide components of chondrules

Instrumental and radiochemical neutron activation analysis is used to determine the concentrations of 14 siderophile and other nonlithophilic elements in 31 chondrules from the extremely unequilibrated chondrite Semarkona. The results are presented in tables and graphs, characterized in detail, and compared with the results obtained for lithophile elements in the same samples by Grossman and Wasson (1983). The elements studied are found to be significantly more fractionated than the lithophile elements, with variations in chondrule/whole-rock abundances of up to a factor of 1000, a mean ratio of 0.2, and differences between Ni-rich and Ni-depleted chondrules. It is argued that the metal and sulfides in the chondrules represent the composition of the solar nebula before chondrule formation and already contained the siderophile and chalcophile elements, although some Fe was contained in silicates along with Ni, Co, Au, Ge and Se. The segregation of metals during a molten stage is considered of minor importance.

Grossman, J. N.↗
NASA NTRS1988

Noble metals in mid-ocean ridge volcanism: A significant fractionation of gold with respect to platinum group metals

Hydrothermal precipitates, black smoker particulate, and massive sulphide dredge samples from the Explorer Ridge on the Juan de Fuca Plate and the TAG hydrothermal area on the Mid-Atlantic Ridge were analyzed for selected noble metals including Au, Ir and Pd by radiochemical neutron activation analysis. The preliminary results indicate that gold contents may reach the ppm range although values in the neighborhood of 100 to 200 ppb are more typical. The platinum group elements (PGE) represented by Ir and Pd are typically less than 0.02 ppb and less than 2 ppb respectively. These abundances represent a significant enrichment of gold relative to the PGE in comparison with average noble metal abundances in mid-ocean ridge basalts (MORB). A partial explanation of this distinctive fractionation can be found in the concepts of sulfur-saturation of basic magma in mid-ocean ridge (MOR) settings, and the origin of MOR hydrothermal fluids. Experimental and petrological data suggest that MORBs are sulfur-saturated at the time of magma generation and that an immiscible sulfide component remains in the mantle residue. Hence, MORBs are noble metal-poor, particularly with respect to PGE. Consequently, black smoker fluids can be expected to reflect the low Ir and Pd contents of the rock column. The average Au content of MORB is 1.3 ppb, and so the rock column is not significantly enriched in Au. The generation of fluids which precipitate solids with 200 ppb Au is apparently dependent on highly efficient fluid chemistry to mobilize Au from the rock column, high Au solubility in seawater hydrothermal fluids and efficient precipitation mechanisms to coprecipitate Au on Fe, Zn and Cu sulfides. Significant differences in these parameters appear to be the ultimate cause of the strong Au-PGE fractionation in the MOR setting. It does not appear from the current data base that MOR hydrothermal fluids are significant contributors to the Ir enrichment seen in Cretaceous-Tertiary boundary sediments.

Crocket, James H.↗
NASA NTRS1988

Cumberland Falls chondritic inclusions. III - Consortium study of relationship to inclusions in Allan Hills 78113 aubrite

The contents of Ag, Au, Bi, Cd, Co, Cs, Ga, In, Rb, Sb, Se, Te, Tl, U, and Zn in large chondritic clasts from the Cumbersand Falls aubrite were determined by radiochemical neutron activation analysis, and the results, together with the results of a mineralogical investigation, were compared with respective data obtained for three primitive inclusions from the ALH A78113 aubrite. The results indicated that the clasts from both aubrite sources constitute a single chondritic suite. The analyses data, together with the results of thermoluminescence data for Cumberland Falls chondritic inclusions and achondritic host, indicate that inclusions in Cumberland Falls and in ALH A78113 aubrite represent a primitive chondrite sample suite whose properties were established during primary nebular accretion and condensation over a broad redox range.

Lipschutz, Michael E.↗
NASA NTRS1989

Lunar meteorites - Siderophile element contents, and implications for the composition and origin of the moon

Data for 10 siderophile elements in all of the known lunar meteorites except for Y793274 are reported. Bulk compositional data for Ni, Ge, Cd, Re, Os, Ir, and Au were obtained from radiochemical neutron activation analysis (Warren et al., 1986). Data for Fe, Co, and Zn, and additional data for Ni, Ir, and Au were obtained by instrumental neutron activation analysis (Kallemeyn et al., 1988). Except for the case of Au in Y791197, there was good agreement between the results obtained by the two methods. The differences observed between the lunar-meteoritic regolith samples and central nearside highlands regolith samples are discussed.

Warren, Paul H.↗
NASA NTRS1991

Chemical studies of H chondrites. III - Regolith evolution of the Fayetteville chondrite parent

Radiochemical neutron concentration analysis was used to determine Ag, Au, Bi, Cd, Co, Cs, Ga, In, Rb, Sb, Se, Te, Tl, and Zn contents in consortium samples of solar gas and track-rich dark matrix. Data obtained confirmed that the matrix is chemically homogeneous. Most dark clasts had similar mean trace element concentrations as the matrix but were compositionally much more heterogeneous. It is concluded that material incorporated with soil and compacted to form the dark portion of Fayetteville included soil-melt, the odd C2M fragment, and dark and light clasts which escaped comminution.

Xiao, Xiaoyue↗
NASA NTRS1995

Chemical studies of H chondrites. 6: Antarctic/non-Antarctic compositional differences revisited

We report data for the trace elements Au, Co, Sb, Ga, Rb, Ag, Se, Cs, Te, Zn, Cd, Bi, T1, and In (ordered by putative volatility during nebular condensation and accretion) determined by radiochemical neutron activation analysis of 14 additional H5 and H6 chondrite falls. Data for the 10 most volatile elements (Rb to In) treated by the multivariate techniques of linear discriminant analysis and logistic regression in these and 44 other falls are compared with those of 59 H4-6 chondrites from Antarctica. Various populations are tested by the multivariate techniques, using the previously developed method of randomization-simulation to assess significance levels. An earlier conclusion, based on fewer examples, that H4-6 chondrite falls are compositionally distinguishable from the Antarctic suite is verified by the additional data. This distinctiveness is highly significant because of the presence of samples from Victoria Land in the Antarctic population, which differ compositionally from falls beyond any reasonable doubt. However, it cannot be proven unequivocally that falls and Antarctic samples from Queen Maud Land are compositionally distinguishable. Trivial causes (e.g., analyst bias, weathering) cannot explain the Victoria Land (Antarctic)/non-Antarctic compositional difference for paradigmatic H4-6 chondrites. This seems to reflect a time-dependent variation of near-Earth meteoroid source regions differing in average thermal history.

Wolf, Stephen F.↗
NASA NTRS1986

Radiocarbon tracer measurements of atmospheric hydroxyl radical concentrations

The usefulness of the C-14 tracer in measurements of atmospheric hydroxyl radical concentration is discussed. The apparatus and the experimental conditions of three variations of a radiochemical method of atmosphere analysis are described and analyzed: the Teflon bag static reactor, the flow reactor (used in the Wallops Island tests), and the aircraft OH titration reactor. The procedure for reduction of the aircraft reactor instrument data is outlined. The problems connected with the measurement of hydroxyl radicals are discussed. It is suggested that the gas-phase radioisotope methods have considerable potential in measuring tropospheric impurities present in very low concentrations.

Campbell, M. J.↗
DOE OSTI2021

Measuring Hydroxylammonium, Nitrate, and Nitrite Concentration with Raman Spectroscopy for 238 Pu Supply Program

Optical spectroscopy has great potential to improve the timeliness of important analytical measurements for the 238 Pu Supply Program by enabling real-time analysis of process solutions within radiochemical hot cells. Hydroxylammonium (H 3 NOH + ]), nitrate (NO 3 - ), and nitrite (NO 2 - ) are three important molecular species present in multiple aqueous streams throughout the program’s flow sheet. The concentration of each species normally goes uncharacterized during processing. However, rapid quantification may benefit the program because uncertainties in kinetic redox expressions describing hydroxylammonium (HA) and nitrite reactions with Np and Pu leads to uncertainty in process model predictions for solvent extraction runs. HA concentration is normally quantified using ion chromatography, a technique that requires diluted grab samples taken out of the hot cell and analyzed off-line. Here we evaluate Raman spectroscopy for determining the concentration of H 3 NOH + , NO 3 - , and NO 2 - in benchtop tests to determine limits of detection. We also consider the possibility of using Raman spectroscopy in both glove box and hot cell environments for rapid analysis and pinpoint additional development opportunities needed to make this application successful.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2025

Characterization of Tank 9H Annulus Sample in Support of Residual Material Inventory Determinations

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Statistical analysis of the performance and long-term stability of unquenched LSC standards ( 3 H, 14 C) used for radiochemical measurements

Multiple sets of toluene-based unquenched standards, procured over the last 3 decades, were analyzed to determine their stability over time. A statistical analysis was performed to provide insight into the variability for tSIE and counting efficiency measurements of 3 H and 14 C isotopes. Our data suggests that standards remain viable even 30 years after the manufacturer’s recommended expiration date. Overall, these standards have shown no statistically significant sign of performance degradation. We have proven through statistical analysis that these standards can provide comparable performance over time well past their manufactured expiration date.

LSC standards↗
DOE OSTI2021

Chemometrics and Experimental Design for the Quantification of Nitrate Salts in Nitric Acid: Near-Infrared Spectroscopy Absorption Analysis

Implementing remote, real-time spectroscopic monitoring of radiochemical processing streams in hot cell environments requires efficiency and simplicity. The success of optical spectroscopy for the quantification of species in chemical systems highly depends on representative training sets and suitable validation sets. Selecting a training set (i.e., calibration standards) to build multivariate regression models is both time- and resource-consuming using standard one-factor-at-a-time approaches. This study describes the use of experimental design to generate spectral training sets and a validation set for the quantification of sodium nitrate (0–1 M) and nitric acid (0.1–10 M) using the near-infrared water band centered at 1440 nm. Partial least squares regression models were built from training sets generated by both D- and I-optimal experimental designs and a one-factor-at-a-time approach. The prediction performance of each model was evaluated by comparing the bias and standard error of prediction for statistical significance. D- and I-optimal designs reduced the number of samples required to build regression models compared with one-factor-at-a-time while also improving performance. Models must be confirmed against a validation sample set when minimizing the number of samples in the training set. The D-optimal design performed the best when considering both performance and efficiency by improving predictive capability and reducing number of samples in the training set by 64% compared with the one-factor-at-a-time approach. The experimental design approach objectively selects calibration and validation spectral data sets based on statistical criterion to optimize performance and minimize resources.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2024

Minimum Detectable Intakes and Doses for Uranium Bioassays—Comparison between Alpha Spectrometry and ICP-MS

Naturally occurring uranium complicates monitoring for occupational exposures. There are several retroactive methods that can be used to monitor for occupational exposures, with benefits and drawbacks to each. Analysis of uranium in urine by mass spectrometry and alpha spectrometry is compared, and methods of determining an occupational exposure are presented. Furthermore, the minimum detectable concentrations from each analysis and a method for intake determination based on the analytical results are compared for various solubility types and mixtures. Mass spectrometry with radiochemical separation was found to be the most sensitive analysis for detecting occupational exposures to anthropogenic mixtures based on minimum detectable doses calculated from the proposed method for intake determination.

bioassay↗
NASA NTRS1976

Chemical fractionations in meteorites. IX - C3 chondrites

Radiochemical neutron activation is applied to the analysis of four C3V chondrites and three C3O chondrites for 17 trace elements (U, Re, Ir, Ni, Au, Sb, Ge, Ag, Rb, Cs, Bi, Tl, Br, Se, Te, In, and Cd). It is shown that both classes exhibit a typical chondritic step pattern, reflecting loss of volatiles during chondrule formation. It appears that the H2S/H2 ratio is the key variable to account for the condensation of chalcophile elements as a function of H2S. C3O's seem to have condensed in a region where enough metallic Fe was present to buffer the H2S pressure, whereas C3V's condensed in a more oxidized region where H2S was in excess. Accretion temperatures for both subclasses is determined. Sb and Au show variable depletion, presumably reflecting variable loss during chondrule formation.

Anders, E.↗
DOE OSTI2022

Cell G 7606A Mockup Measurement Analysis Methods and Results

The production of research isotopes at the Radiochemical Engineering Development Center (REDC) invariably leads to the accumulation of radioactive waste. Storage of this waste onsite at ORNL serves as an interim solution prior to shipment to long term storage facilities, however onsite capacity is limited. Proper characterization of the activity of waste products is essential for determining the appropriate waste stream and, ultimately, mitigating the cost of disposal. This is typically done via gamma spectrometry and use of the In-Situ Object Counting System (ISOCS), a software package from Mirion that serves as an accepted community standard. However, variability in the contents, density, and activity distribution in waste containers can introduce large errors in ISOCS quantification. A measurement campaign using a mockup of the proposed setup in Cell G seeks to quantify the magnitude and source of these systematic errors. Analysis of this data will guide the creation of ISOCS geometry templates and measurement methods designed to minimize overall uncertainty in reported activities.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1974

Trace geochemistry of lunar material

The lunar samples from the Apollo 16 and 17 flights which were analyzed include soil, igneous rock, anorthositic gabbro, orange soil, subfloor basalt, and norite breccia. Up to 57 elements including majors, minors, rare earths and other trace elements were determined in the lunar samples. The analytical techniques used were spark source mass spectrometry and neutron activation analysis. The latter was done either instrumentally or with group radiochemical separations. The differences in abundances of the elements in lunar soils at the various sites are discussed. With regard to the major elements only Si is about the same at all the sites. A detailed analysis which was performed on a sample of the Allende meteorite is summarized.

Morrison, G. H.↗
DOE OSTI2022

Irradiation of Sintered Mo Disks with Presence of Organic Impurities in He Gas Flow

Argonne National Laboratory (Argonne) is assisting NorthStar Medical Technologies in the development of a domestic supply of 99 Mo. Specifically, the present study focuses on the production of 99 Mo-feed solution used by the RadioGenix™ 99m Tc generator. During the target-irradiation phase of production, impurities can potentially be introduced into the feed, and can lead to disturbance of ligand- 99m Tc complexation chemistry and contamination of the final radiopharmaceutical that directly interacts with the patient. To address this issue, Argonne performed irradiations and chemical processing to identify whether the potential contamination of He flow with hydrocarbon oil during irradiation affects the radiochemical purity of the final K 2 MoO 4 (K 2 TcO 4 ) in 5M KOH solution. To mimic the conditions of real irradiation at NorthStar, Argonne used its electron linear accelerator and Van de Graaff facilities, heated the target and oil source to >800°C, and controlled oxygen in the presence of He during irradiation. Following irradiation, scanning electron microscopy (SEM) and carbon analysis (CA) were used to detect carbon contamination on the solid targets. The radiochemical purity of the dissolved targets was studied via thin-layer paper chromatography (TLC). As a result of these experiments, small regions of the surface of some irradiated disks were found to be high in carbon, but the total carbon content was still negligible in comparison to the reference sample, which had experienced no irradiation or contact with oil. The summarized results from the SEM, CA, and TLC tests lead to the conclusion that even an excess of oil and heating during irradiation do not affect the radiochemical purity of the final product.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗