Improved instrumental techniques, including isotopic analysis, applicable to the characterization of unusual materials with potential relevance to aerospace forensics

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Abstract

The problem of precise characterization, analysis, and eventual identification of unknown materials arises in many fields and takes many forms, depending on the nature of the substances under study. In the first part of this paper we review common, modern mass spectrometry techniques applied to such studies. We also give an overview of improvements made to these technologies in recent years by Silicon Valley companies and other teams focused on precise biomedical research dependent upon sensitive techniques, yet applicable to a wide range of non-biological materials. In the second and third parts of the paper we review practical experiences applying these techniques to the simplest case of the characterization of solid materials (as opposed to liquids or gases) and comparing our results with previously undertaken isotopic analysis. In particular, we describe our correlations of that analysis with the patterns described by witnesses in a well-documented, still-unexplained incident, initially thought to be of aerospace origin, which gave rise to the deposition of unknown material, and by the investigators who handled it in the field and the laboratory. The lessons from this specific investigation are applicable to a wider range of issues in reverse engineering of complex, esoteric materials, and aerospace forensics.

Introduction

The problem of precise characterization, analysis, and eventual identification of unknown materials arises in many fields -- ranging from archaeology to meteoritics, medicine, law enforcement, nuclear forensics, space exploration and national (US and foreign) intelligence agencies. In materials analysis of metals and other inorganics, the approach can take many forms, depending on the nature of the substances under study. In general, one starts with basic constituents such as elemental composition, moving onto studies of internal structure if any.

In the first part of this report, we review common analytic procedures, including modern mass spectrometry, X-Ray spectroscopy, and certain other techniques that are often initially applied for such studies. We also provide an overview of improvements made to one of these technologies in recent years by investigators that focused on precise biomedical research with sensitive techniques yet are still applicable to a wide range of non-biological materials. This development was driven by that fact that most materials are not ‘uniform’ in their composition and therefore techniques that allow for 2D and 3D analysis of materials are key to both understanding as well as quality control.

For example, an insight brought from the biological research arena is that spatial patterns (for instance, of cells) in a tissue are critical determinants of outcomes in disease states (whether certain immune cell types are within a given radius of a tumor or pathogen). Spatial component organization is key as well in design of microelectronic circuitry. As such, in the analysis of novel materials whose function will depend on local changes in elemental composition (wiring or semiconductors), the use of spatially sensitive instrumentation adds great value. In addition, while isotopes of elements are often considered equal in functional attributes for most purposes, subtle distinctions in properties of isotopes relative to spin states of nuclei, utility in quantum entanglement systems, and even pharmaceutical effects have been apparent in recent years (detailed below).

In the second and third parts of this report we review practical experience applying some of these techniques to a simple case of the characterization of a solid material (as opposed to liquids or gases) while comparing our results with previously undertaken isotopic and elemental analysis.

We describe correlations of that analysis with the patterns described by witnesses in a well-documented, still-unexplained incident, initially thought to be of aerospace origin, which gave rise to the deposition of an unknown material, and by the investigators who handled it in the field and in the laboratory. The lessons from this specific investigation are applicable to a wider range of issues in reverse engineering of complex, esoteric materials, and aerospace forensics.

We apply these insights to a case of a material derived from an unidentified aerial object as observed by multiple independent witnesses. We apply the standard, and new, techniques as outlined herein as an example of how the analysis of such materials can be addressed. We detail the elemental and spatial differences in elemental and isotopic composition of subsamples from the parent sample CB_JV-1 at 50 nm resolution. The results show differences in the elemental distribution based on 5 subsample grains, suggesting the parent sample is inhomogeneous. For each of the subsamples the elemental composition was homogeneous to a depth of ∼50 nm. Notably, there were no significant isotopic differences from terrestrial normal in the subsamples, and thus the overall sample could have been made with terrestrial-derived materials. That said, the CB_JV-1 sample itself remains of unknown provenance or function.

Section snippets

Basic approaches for the initial characterization of unknown materials

There are multiple technologies for determining the chemical makeup of complex materials. The analytic approach that is to be taken is largely determined by the general nature of the material under analysis. With materials of completely unknown makeup, and starting from the smallest scale, one can begin with identifying the elements, such as hydrogen, carbon, iron, copper, and so on, and determining their relative abundances within a sample. While for most analytic purposes the isotopes of a

Investigating unknown material collected in the field: A case study

Elemental and isotopic analysis has proven of value in the study of material recovered from disintegrating aeronautical or astronomical objects, or from residue deposited on earth following an observation of an unknown phenomenon. In such cases it is essential to distinguish between natural and manufactured material and, in the latter case, to obtain information about the process that led to the creation of the recovered sample, and its potential purpose.

While geologists and astronomers are

Advanced analytical methods applicable to exceptional physical events

The material recovered at Council Bluffs consists of three components: solid metal, slag, and white ash inclusions in the slag. In the previous section we have mentioned the results of the analysis at the Ames Laboratory, which examined all three of those by X-Ray fluorescence, electron beam microprobe, and emission spectroscopy, under the supervision of Mr. Edward DeKalb.

Speculative conclusions

We have outlined current trends in advanced materials analysis, as applied to solid samples collected in the field, with a view to determine their nature, structure, and potential purpose. Our experience with the Council Bluffs case study shows how difficult such a determination can be, even when abundant evidence is collected within minutes of an event, supported by reliable testimony from multiple witnesses and in well-defined meteorological conditions.

Summary

Because of the clarity, abundance and timeliness of the testimony, and the open attitude of local police and fire investigators in the Council Bluffs case, we were able to investigate the event with a high degree of certainty as to chain of custody around the material obtained. While this study verified the prior findings in terms of elemental composition and “natural” isotope content, we additionally found that there was local homogeneity of the samples to the degree measured, but considerable

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments

The authors wish to thank the following persons who contributed to the documentation of the Council Bluffs case and to its scientific investigation: Mr. Robert Allen, journalist, and amateur astronomer; Dr. Michael Angelo, IonPath, Inc.; Mr. Randy Fitzgerald, The Reader's Digest; Mr. Robert Hansen, Director, Ames Laboratory, Iowa State University; Mr. Richard Masilko, investigator, Omaha, Nebraska; Mr. Jack Moore, assistant fire chief, Council Bluffs; Officer Dennis Murphy, Council Bluffs

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