Richard E. Whipple

Standoff Detection of High Explosive Materials at 50 Meters in Ambient Light Conditions Using a Small Raman Instrument

We have designed and demonstrated a standoff Raman system for detecting high explosive materials at distances up to 50 meters in ambient light conditions. In the system, light is collected using an 8-in. Schmidt–Cassegrain telescope fiber-coupled to an f/1.8 spectrograph with a gated intensified charge-coupled device (ICCD) detector. A frequency-doubled Nd: YAG (532 nm) pulsed (10 Hz) laser is used as the excitation source for measuring remote spectra of samples containing up to 8% explosive materials. The explosives RDX, TNT, and PETN as well as nitrate- and chlorate-containing materials were used to evaluate the performance of the system with samples placed at distances of 27 and 50 meters. Laser power studies were performed to determine the effects of laser heating and photodegradation on the samples. Raman signal levels were found to increase linearly with increasing laser energy up to ∼3 × 106 W/cm2 for all samples except TNT, which showed some evidence of photo- or thermal degradation at higher laser power densities. Detector gate width studies showed that Raman spectra could be acquired in high levels of ambient light using a 10 microsecond gate width.

Nuclear forensics in law enforcement applications

Over the past several years, the Livermore Forensic Science Center has conducted analyses of nuclear-related samples in conjunction with domestic and international criminal investigations. Law enforcement officials have sought conventional and nuclear-forensic analyses of questioned specimens that have typically consisted of miscellaneous metal species or actinide salts. The investigated activities have included nuclear smuggling and the proliferation of alleged fissionable materials, nonradioactive hoaxes such as “Red Mercury,” and the interdiction of illegal laboratories engaged in methamphetamine synthesis.

Analysis of tetrodotoxin

Abstract Law enforcement personnel interdicted an illegal shipment of a chemical suspected to be an illicit drug. However, literature within the package indicated that the substance was actually tetrodotoxin, a potent marine neurotoxin. Analyses of the questioned samples by gas chromatography–mass spectrometry revealed no evidence for the presence of illicit drugs, but this technique was ineffectual for the identification of tetrodotoxin. Direct-inlet-probe mass spectrometry was likewise unable to characterize the chemical identity of the subject material. Electrospray-ionization mass spectrometry was implemented to successfully identify the interdicted substance as tetrodotoxin.

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.

On-site Analysis of Explosives in Various Matrices

Lawrence Livermore National Laboratory (LLNL) has developed several different strategies and technologies for the on-site detection of explosives. These on-site detection techniques include a colorimetric test, thin layer chromatography (TLC) kit and portable gas chromatography mass spectrometer (GC/MS). The screening of suspicious containers on-site and the search for trace explosive residue in a post-blast forensic investigation are of great importance. For these reasons, LLNLs Forensic Science Center has developed a variety of fieldable detection technologies to screen for a wide range of explosives in various matrices and scenarios. Ideally, what is needed is a fast, accurate, easy-to-use, pocket-size and inexpensive field screening test for explosives.

Search for evidence of nuclear involvement in the fatal explosion of a “cold fusion” experiment

Forensic analyses of debris from the fatal explosion of an electrochemical “cold fusion” cell at SRI International were conducted at LLNL at the request of Cal-OSHA. One investigation focused on the possibility of conventional nuclear reaction mechanisms contributing to the total energy inventory of the incident. Selected metal components of the electrolysis apparatus were subjected to nondestructive γ-ray spectrometry with high-sensitivity, low-background Ge detector systems. The anticipated analytes in these studies were radioactivation products potentially induced in the explosion residue by either fast or thermal neutrons. The results of this investigation were negative within the temporal constraints of the incident and the analytical sensitivities of the instrumentation.

On-Site Sample Work-Up Procedures to Isolate Chemical Warfare Related Compounds using Solid Phase Extraction and Solid Phase Microextraction Technology

The rapid preparation and accurate analysis in the field of suspect samples is most important for on-site investigations relevant to the planned Chemical Weapons Convention (CWC) inspections. Sample preparation becomes the limiting factor and one of the most critical aspects of the challenge inspection. The primary aim of the analysis is to detect the presence of undeclared chemicals subject to control by the Convention.

Comprehensive forensic analyses of debris from the fatal explosion of a "cold fusion" electrochemical cell

Selected components of explosion debris from the SRI International incident of January 2, 1992 were subjected to forensic analyses to elucidate potential causes of, or contributing factors to, the explosion. Interrogation of the debris encompassed nuclear, chemical, physical, and materials investigations. Nuclear studies for the determination of tritium and neutron-activation products in stainless steel and brass were conducted. No evidence for signature species indicative of orthodox nuclear events was detected. The inorganic and particulate analyses were likewise negative with respect to residues of unexpected chemical species. Such target compounds included conventional explosives, accelerants, propellants, or any exceptional industrial chemicals. Materials characterization identified the type of stainless steel used in the manufacture of the electrolytic cell as one relatively high in Mo concentration, probably type 316. Metallurgical analyses of the cell vessel wall and its detached base provided no evidence of corrosion or hydrogen embrittlement, leaving only ductile failure of the weld as contributing to the incident. The weld was found to have missed the center-line of the step joint, and the average penetration of the weld was measured to be 54%. The GC-MS analyses of trace organic components in the explosion debris provided a most interesting result. Although no evidence of organic explosives, oxidizers, or other unusual compounds was detected, the presence of an organic oil in the interior of the electrochemical cell was established. It is likely that the source of this oil was lubricating fluid from machining the metal cell components.(ABSTRACT TRUNCATED AT 250 WORDS)

Portable thin layer chromatography for field detection of explosives and propellants

A field deployable detection kit for explosives and propellants using thin layer chromatography (TLC) has been developed at Lawrence Livermore National Laboratory (LLNL). The chemistry of the kit has been modified to allow for field detection of propellants (through propellant stabilizers), military explosives, peroxide explosives, nitrates and inorganic oxidizer precursors. For many of these target analytes, the detection limit is in the μg to pg range. A new miniaturized, bench prototype, field portable TLC (Micro TLC) kit has also been developed for the detection and identification of common military explosives. It has been demonstrated in a laboratory environment and is ready for field-testing. The kit is comprised of a low cost set of commercially available components specifically assembled for rapid identification needed in the field and identifies the common military explosives: HMX, RDX, Tetryl, Explosive D or picric acid, and TNT all on one plate. Additional modifications of the Micro TLC system have been made with fluorescent organosilicon co-polymer coatings to detect a large suite of explosives.