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Evaluation of Properties for Microsample Identification

A study was conducted to determine if individual particle characteristics could be used to identify particles of interest, sub-samples, from bulk post-detonation debris. Three archived post-detonation debris samples were used for this effort. Particles from these samples were identified as active (produced fission tracks), and inactive (did not produce fission tracks), as the first defining characteristic. Morphology was the secondary characteristic to select particles for further study, i.e. spherical/non-spherical. Once particles were identified and isolated, they were characterized by optical microscopy for size in µm, number of fission tracks, morphology, transmitted light color, and reflected light color. Particles were then analyzed by scanning electron microscopy for morphology, elemental content, and compound identification. Raman spectroscopy was attempted on five particles with indeterminate results due to environmental mixing (heterogeneity) during the events of particle formation. Once all non-destructive analyses were completed all particles were analyzed by thermal ionization mass spectrometry to determine isotopic atom percents of plutonium and uranium, and an estimate of atoms of plutonium and uranium in each particle. An estimate of the ratio of uranium to plutonium was also obtained (U/Pu). Data analytics of the data from the particles showed that combining characteristics of the particles have a high probability of identifying particles of interest from bulk post-detonation debris samples. Please note that this version of the report is an abridged version of the full report (Wagnon et al. 2025) that has been edited to be appropriate for public release.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA

Evaluation of dried blood spot sampling for verification of exposure to chemical threat agents

Abstract Purpose Exposure to chemical threat agents (CTAs), including nerve agents, the vesicating agent sulfur mustard, and opioids, remains a significant threat to warfighter and civilian populations. Definitive analytical methods to verify exposure to CTAs require shipping refrigerated or frozen biomedical samples to reference laboratories for analysis. Logistical and financial burdens arise as the transport of biomedical samples is subject to strict restrictions and complex packaging, which, if done incorrectly, can lead to sample deterioration. The use of dried blood spot (DBS) sampling could provide operational improvements for collecting, storing, and shipping important forensic samples. Therefore, this effort focuses on developing DBS techniques with Mitra® 30-µL volumetric absorptive microsampling (VAMS®) devices for use in CTA exposure verification. Methods VAMS® devices were loaded and dried with human whole blood that was exposed to the metabolites pinacolyl methylphosphonic acid (PMPA), ethyl methylphosphonic acid (EMPA), 1,1’sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE), norfentanyl, norcarfentanil, norsufentanil, and norlofentanil. Following extraction from the VAMS® devices, metabolites were detected using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The methods were validated for performance by assessing sensitivity, precision, accuracy, and recovery. Results These methods were sensitive to 1 ng/mL for SBMSE, 0.5 ng/mL for PMPA, EMPA, and norfentanyl; 0.1 ng/mL for norlofentanil, and 0.05 ng/mL for norsufentanil and norcarfentanil. All methods met acceptable precision and accuracy criteria with favorable recovery. Conclusions These results demonstrated the utility of VAMS® in stabilizing human whole blood and show promise as an improved collection method for verification of exposure to various CTAs.

Toxicology

A Methodology for determining optimal milling parameters for low-taper microtensile sample production

Femtosecond lasers are beginning to see an increase in interest for industrial and high throughput microsample milling applications. Despite this, much of the literature regarding removal rate studies for ultrashort pulse laser milling continues to focus on single-pulse or similar experiments that have a very small time on target. The material volume removal rates of femtosecond milling can vary wildly depending on parameters like laser scan speed, hatch spacing, z-axis step size, and pulses on the material. Currently, there is no established methodology for determining the optimal values of these parameters for micromilling applications. This methodology was developed in this study. The methodology consists of a pulse study, a repeat study, and a z-step study that will return the milling parameters that resulted in the largest volume removal rate for the laser used for this research. The methodology was created for the laser system used in this study, and was tested on 316 Stainless Steel, but was developed in such a way that it may be adapted to any material, and with some tweaking of variables might be used in other laser systems. The laser system used in this study utilizes a novel positioning stage that introduces 6 degrees of freedom to the translation of laser samples, being able to tilt and move in all three axes. Using both the developed methodology and the unique capabilities of the laser microtensile samples were produced with taper angles of <1° in 316 Stainless Steel.

Barker, Zachary Wayne