Patrick Grant

Chemical and elemental comparison of two formulations of oleoresin capsicum

In-custody deaths following the application of pepper spray weaponry by law enforcement personnel have increased in California over the last few years. Oleoresin capsicum (OC), an oily extract of hot peppers, is the active ingredient in the spray, but little detailed information on product mixtures is available. Since OC extracts contain a multitude of natural compounds at irregular concentrations, there could be considerable, variation in overall chemical composition among the different formulations of both natural and synthetic OC preparations. This was confirmed by organic and inorganic analyses performed on OC sprays produced by two manufacturers licensed for distribution within the state of California. The results indicated that the differences could lead to considerable inconsistency in weapon effectiveness, and suggested that more comprehensive studies are warranted.

Optimum methamphetamine profiling with sample preparation by solid-phase microextraction.

Solid-phase microextraction (SPME) is a relatively new technique in which a small, polymer-coated fiber is employed to extract volatile and semivolatile organic compounds from the sealed headspace above a questioned sample. SPME, coupled with gas chromatography/mass spectrometry (GC/MS), was used to characterize impurities in illicit methamphetamine samples. Trace impurities present in a specimen were tentatively identified using mass-spectral databases and included 1,2-dimethyl-3-phenyl-aziridine (indicating synthesis via a halogenated ephedrine intermediate), ethyl vanillin (a flavoring compound), and caffeine (a stimulant used as cutting agent). The types and numbers of organic compounds sampled by SPME were compared with those collected by various solvent extraction protocols. In addition to unambiguously confirming the presence of methamphetamine, SPME-GC/MS analyses detected approximately 30 more organic analytes than were found by GC/MS following the ethyl acetate extraction method adopted by the United Nations International Drug Control Programme. SPME-GC/MS is a superior method for generating material fingerprint profiles in methamphetamine samples. The detection and characterization of increased points of comparison in drug samples provide more detailed chemical signatures for both intelligence and operational information.

Radiochemical Determination of Inertial Confinement Fusion Capsule Compression at the National Ignition Facility

We describe a radiochemical measurement of the ratio of isotope concentrations produced in a gold hohlraum surrounding an Inertial Confinement Fusion capsule at the National Ignition Facility (NIF). We relate the ratio of the concentrations of (n,γ) and (n,2n) products in the gold hohlraum matrix to the down-scatter of neutrons in the compressed fuel and, consequently, to the fuels areal density. The observed ratio of the concentrations of (198m+g)Au and (196g)Au is a performance signature of ablator areal density and the fuel assembly confinement time. We identify the measurement of nuclear cross sections of astrophysical importance as a potential application of the neutrons generated at the NIF.

Application of Visible/Near-Infrared Reflectance Spectroscopy to Uranium Ore Concentrates for Nuclear Forensic Analysis and Attribution

Uranium ore concentrates (UOCs) are produced at mining facilities from the various types of uranium-bearing ores using several processes that can include different reagents, separation procedures, and drying conditions. The final UOC products can consist of different uranium species, which are important to identify to trace interdicted samples back to their origins. Color has been used as a simple indicator; however, visual determination is subjective and no chemical information is provided. In this work, we report the application of near-infrared (NIR) spectroscopy as a non-contact, non-destructive method to rapidly analyze UOC materials for species and/or process information. Diffuse reflectance spectra from 350 to 2500 nm were measured from a number UOC samples that were also characterized by X-ray diffraction. Combination and overtone bands were used to identify the amine and hydroxyl-containing species, such as ammonium uranates or ammonium uranyl carbonate, while other uranium oxide species (e.g., uranium trioxide [UO3] and triuranium octoxide [U3O8]) exhibit absorption bands arising from crystal field effects and electronic transitions. Principal component analysis was used to classify the different UOC materials.

Forensic Analyses of Suspect Illicit Nuclear Material

A small metal sample, alleged to be a substance that could substitute for highly enriched uranium in a nuclear weapon, was subjected to qualitative and quantitative forensic analyses using methods of materials science, radioisotopic chemistry, inorganic chemistry, and organic chemistry. The specimen was determined to be moderately pure Sc, likely derived from a uranium refining operation. Although no fissionable species or weaponization signatures were detected, the sample did exhibit some unusual properties. These anomalies included lanthanide fractionation, with concentrations of Dy, Ho, and Er elevated by factors greater than 100 over normal levels, and the presence of long, odd-chain fatty acids.

A possible chemical explanation for the events associated with the death of Gloria Ramirez at Riverside General Hospital

The events associated with the death of Gloria Ramirez at Riverside General Hospital on 19 February 1994 have been portrayed as a major medical mystery. A potential chemical explanation for this incident has been developed. The hypothetical scenario depends upon the oxidation of a common solvent, dimethyl sulfoxide, through dimethyl sulfone to dimethyl sulfate. The latter compound is a volatile and highly toxic agent that can be quite hazardous to humans in small amounts. It is also environmentally nonpersistent. Much of the mystery surrounding the circumstances at the hospital may be explainable if this postulated metabolic pathway took place at the time of the emergency room incident. Although dimethyl sulfate was not detected in any analyses pertinent to this event, there are plausible scientific explanations to account for that fact. The sulfate anion, a hydrolysis product of dimethyl sulfate, was measured at an appreciably elevated concentration in Ramirez blood. The descriptions of the symptoms of the hospital-staff victims appear quite consistent with dimethyl sulfate exposures. This paper attempts to make some sense of the reported data and eyewitness accounts, and perhaps provide new insight for any future research that could further explain this reported occurrence of toxic exposure.

Proper Assessment of the JFK Assassination Bullet Lead Evidence from Metallurgical and Statistical Perspectives

ABSTRACT: The bullet evidence in the JFK assassination investigation was reexamined from metallurgical and statistical standpoints. The questioned specimens are comprised of soft lead, possibly from full‐metal‐jacketed Mannlicher‐Carcano (MC), 6.5‐mm ammunition. During lead refining, contaminant elements are removed to specified levels for a desired alloy or composition. Microsegregation of trace and minor elements during lead casting and processing can account for the experimental variabilities measured in various evidentiary and comparison samples by laboratory analysts. Thus, elevated concentrations of antimony and copper at crystallographic grain boundaries, the widely varying sizes of grains in MC bullet lead, and the 5–60u2003mg bullet samples analyzed for assassination intelligence effectively resulted in operational sampling error for the analyses. This deficiency was not considered in the original data interpretation and resulted in an invalid conclusion in favor of the single‐bullet theory of the assassination. Alternate statistical calculations, based on the historic analytical data, incorporating weighted averaging and propagation of experimental uncertainties also considerably weaken support for the single‐bullet theory. In effect, this assessment of the material composition of the lead specimens from the assassination concludes that the extant evidence is consistent with any number between two and five rounds fired in Dealey Plaza during the shooting.

Production and isolation of homologs of flerovium and element 115 at the Lawrence Livermore National Laboratory Center for Accelerator Mass Spectrometry

New procedures have been developed to isolate no-carrier-added (NCA) radionuclides of the homologs and pseudo-homologs of flerovium (Hg, Sn) and element 115 (Sb), produced by 12–15xa0MeV proton irradiation of foil stacks with the tandem Van-de-Graaff accelerator at the Lawrence Livermore National Laboratory Center for Accelerator Mass Spectrometry (CAMS) facility. The separation of 113Sn from natIn foil was performed with anion-exchange chromatography from hydrochloric and nitric acid matrices. A cation-exchange chromatography method based on hydrochloric and mixed hydrochloric/hydroiodic acids was used to separate 124Sb from natSn foil. A procedure using Eichrom TEVA resin was developed to separate 197Hg from Au foil. These results demonstrate the suitability of using the CAMS facility to produce NCA radioisotopes for studies of transactinide homologs.

First fission yield measurements at the National Ignition Facility: 14-MeV neutron fission of 238U

The use of the Solid Radiochemistry diagnostic platform at the National Ignition Facility (NIF) has allowed the development and implementation of the Target Option Activation Device assembly for fielding materials of interest inside the NIF chamber during high yield neutron shots. Preliminary studies with ultra-depleted uranium have allowed for the measurements of fission yields of 238U. Radiochemical procedures were utilized for the separation of fission and reaction products from the target material to provide higher sensitivity measurements. Cumulative fission mass-yields for 32 different isobars, 72xa0≤xa0Axa0≤xa0153, were measured from experiments fielded on two separate NIF shots.

Advanced Techniques in Physical Forensic Science

The techniques and tools of modern physics have long been profitably applied to forensic science. Since the 1900s, forensic scientists have analyzed gunshot residues, examined fired munitions, determined the refractive indices of glass—to name a few of their diverse activities.