Felice Nunziata | Consiglio Nazionale delle Ricerche (CNR) (original) (raw)
X ray fluorescence - Energy Dispersion by Felice Nunziata
Journal of Cultural Heritage, 2005
XRF and micro-Raman stratigraphic microanalyses of fragments of some mural paintings, belonging t... more XRF and micro-Raman stratigraphic microanalyses of fragments of some mural paintings, belonging to the Archaeological Site of Oplonti (Napoli) and the Vigna Barberini site in the Palatino (Roma), were performed. In order to collimate the fluorescence X-rays emitted by the samples, an X-ray polycapillary conic collimator (PCC) has been used in front of the detector. This device arrangement is compact, versatile, and portable. The nature of the pigments, the compositional elements, and the thickness of the fragment layers have been studied. The stratigraphic analysis partially confirms the preparation techniques described by Plinius and Vitruvius; moreover it confirms the hypothesis that the artifacts are not fresco paintings. This work has been conducted within the context of a wider research on the Roman age mural paintings.
Residui dello Sparo _ Gunshot Residues by Felice Nunziata
Forensic Science International
Journal of Forensic Science & Criminology, 2017
Observations by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) of un... more Observations by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) of unfired standard primer material (lead/antimony/barium) are presented from the centerfire cartridge primers of Winchester, Speer and Remington. Also examined by SEM/EDS are the surfaces of thirtytwo gunpowders (GPs) from Winchester, Federal, Hercules, DuPont and Remington. Compounds of sulfur, potassium and barium as well as primer-like particles composed of lead, antimony and barium were found on the surfaces of many of these GPs. The elements of these compounds likely contribute to gunshot residue (GSR) generated by the discharge of a firearm. We introduce the term, ―hybrid GSR‖ which will account for both the contribution to primer GSR by the interior firearm surfaces GSR and the elements associated with GP.
Egyptian Journal of Forensic Sciences 13 (2023), 2023
The forms and compositions of primer gunshot residue (GSR) in shooting cases have been routinely ... more The forms and compositions of primer gunshot residue (GSR) in shooting cases have been routinely analyzed in many crime labs by scanning electron microscope/energy-dispersive X-ray spectroscopy (SEM/EDS). Gunshot residue studies over the last 30 years have identified a contribution by residual GSR from surfaces within the firearm to GSR (the “memory effect”). In this study, we first focus on the GSR compositional differences between target, bore, and cylinder gap for a .22 caliber revolver which has received little attention in the literature. Secondly, we examine the behavior of elements involved in the residual contribution to GSR for a .22 caliber pistol.
Forensic Chemistry Available online 9 January 2023, 100472 In Press, Journal Pre-proofWhat are Jo... more Forensic Chemistry
Available online 9 January 2023, 100472
In Press, Journal Pre-proofWhat are Journal Pre-proof articles?
On the problem of data interpretation in the analysis of iron-containing GSR particles
Author links open overlay panelMarcoRomeoaFeliceNunziatae
https://doi.org/10.1016/j.forc.2023.100472
Get rights and content
Highlights
•
Iron is an element that can be present within a GSR particle;
•
The iron present in a GSR particle can be derived from several sources;
•
Forensic experts hypothesize that the iron may have come from the barrel of the firearm;
•
Several iron particles from the barrel of the firearm and other sources were analyzed;
•
In gunfire with rusty barrels, iron particles aggregate with GSRs in the cooling phase.
Abstract
Many forensic experts hypothesize that iron found in gunshot residues (GSRs) derive from melted iron particles because the steel of the barrel consists mainly of iron. This is a strong hypothesis that deserve careful investigation. To this purpose, we focused our attention on erosion and corrosion mechanism occurring in the barrel that can influence GSRs. A preliminary physicochemical interpretation consistent with the analytical results was presented. Moreover, spectra and images of GSRs originated from the firing of ammunition by firearms having rusty barrels and of iron oxide particles not originated from the firing were analyzed. The obtained results are discussed, taking into account the chemical content and morphology of the observed particles taking in account the context both of the erosion and of the corrosion and of the GSRs formation process
Inorganic gunshot residue (GSR) analysis is carried out by scanning electron microscopy/energy-di... more Inorganic gunshot residue (GSR) analysis is carried out by scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS)
in many forensic laboratories. Characteristic GSR often consists of lead–barium–antimony, commonly associated with sulfur. The strength
of forensic GSR evidence increases when unusual elements are found in residues collected both from the suspect and from the discharged
firearm. The presence of molybdenum in GSR, due to the use of MoS 2 lubricants in firearms, is experimentally demonstrated here for the
first time. The most intense molybdenum X-ray emissions are MoL peaks at 2.3 keV which overlap with PbM and SK families due to the
poor resolution of EDS detectors. When Pb, S, and Mo are allegedly present in the same particle, the reliability of automatic EDS routines is
at risk. Missing identifications or false detections and exclusions may then occur. Molybdenum should be considered as detected only if
MoK emissions meet the peak-to-background ratio minimum requirements. A strategy to spot Mo-containing residues is described,
based on the automated search of MoS 2 , using a new “Sulfur only” class added to the classification scheme, followed by careful manual
review of all GSR particles at an acceleration voltage of 30 kV. Our proposal improves commonly adopted forensic procedures currently
followed in casework.
The surfaces of thirty-one gunpowders (GPs) from Winchester, Federal, Hercules, DuPont, and Remin... more The surfaces of thirty-one gunpowders (GPs) from Winchester, Federal, Hercules,
DuPont, and Remington were examined by scanning electron microscopy/energy
dispersive X-ray spectroscopy. Particles and surface coatings on 22 of the GPs had
compositions of sulfur/potassium/barium or sulfur/potassium detected. Primer-like
particles composed of lead/antimony/barium were found on surfaces of twelve GPs.
Gunpowders from fifteen different lots of Winchester 9 mm Silvertip ® hollow point
cartridges were found to vary in GP type (flake and flattened ball) and associated
inorganic compounds of sulfur/potassium/barium or sulfur/potassium or one with
only potassium. No inorganic particles or coatings were detected on two of these
Winchester GPs. The elements from the inorganic compounds on GPs likely contrib-
ute to gunshot residue generated by the discharge of a firearm.
MERCURY STRUCTURAL SEGREGATION IN RESIDUE OF MERCURY FULMINATE IN RESIDUE OF MERCURY FULMINATE BASED PRIMERS BASED PRIMERS, 2019
In this work we propose the hypothesis that the chemical-physical properties of mercury can deter... more In this work we propose the hypothesis that the chemical-physical properties of mercury can determine its relative evanescence in GSR: in the other words we propose preliminary experimental results from which we derive, in according to thermodynamic laws, an possible explanation in term grain refinement, segregation and diffusion hybrid model.
Journal of Analytical Atomic Spectrometry, 2019
Standard analysis of inorganic gunshot residue aims nowadays at lead, antimony and barium particl... more Standard analysis of inorganic gunshot residue aims nowadays at lead, antimony and barium particles of spherical shape, although other elements are detected that may be indicative of the ammunition brand or interaction with specific materials. Calcium and phosphorus can be present in the particle systems examined. There are two main sources of these elements in gunshot residue: components of the ammunition, e.g. Eley brand .22 long rifle caliber and bone fragments created during contact and close-range shooting. Samples of human bones of various ages and the residue from the interior of spent cartridges of ten different products of Eley brand .22 long rifle caliber ammunition were systematically characterised as reference materials to aid the interpretation of candidate GSR particles detected in evidence samples. We found that Ca : P ratios obtained by means of scanning electron microscopy with energy dispersive X-ray spectrometry from GSR particles larger than about 10 micrometres characterised bone fragments reliably. Although Ca and P may be detected as traces, for smaller (micron and sub-micron) particles the Ca : P ratio is not a reliable indicator of bone material. But in such cases qualitative interpretation taking into account interdisciplinary information can be achieved for forensic purposes. Three case studies encompassing various types and amounts of gunshot residue identified the possibilities and limitations in the differentiation between the potential sources of calcium and phosphorus present in inorganic gunshot residue.
In their first full report on the analysis of GSR by SEM-EDS, Wolten and colleagues stated that t... more In their first full report on the analysis of GSR by SEM-EDS, Wolten and colleagues stated that the great majority of the gunshot residue particles (GSR), between 70 to 100%, have a characteristic morphology thus providing a detection criterion holding significance equal to that provided by the elemental composition. In fact, the particles must have a spherical or spheroidal shape and their surface should appear amorphous, devoid of any crystalline characteristic.
On a gunshot residue three-dimensional roundedness For the proper identification of GSR by SEM/ED... more On a gunshot residue three-dimensional roundedness
For the proper identification of GSR by SEM/EDX, together with a correct and congruent elemental analysis, is also essential to take into account the morphology of the particles and the nature of their surfaces. GSR corpuscles are formed during a rapid solidification process and, having assumed at the liquid state a spherical shape, they maintain this characteristic as solidification occurs. Their surfaces, probably due to a phenomenon of "grain refinement" , should appear completely amorphous at the normal working magnification with no trace of crystalline formations. This principle has been expressed already in 1977 by G.M. Wolten and colleagues in their fundamental work , and has been confirmed over the years by all the experienced scientists of the field including Prof. Carlo Torre and many others until Mar 2016.
Journal of Cultural Heritage, 2005
XRF and micro-Raman stratigraphic microanalyses of fragments of some mural paintings, belonging t... more XRF and micro-Raman stratigraphic microanalyses of fragments of some mural paintings, belonging to the Archaeological Site of Oplonti (Napoli) and the Vigna Barberini site in the Palatino (Roma), were performed. In order to collimate the fluorescence X-rays emitted by the samples, an X-ray polycapillary conic collimator (PCC) has been used in front of the detector. This device arrangement is compact, versatile, and portable. The nature of the pigments, the compositional elements, and the thickness of the fragment layers have been studied. The stratigraphic analysis partially confirms the preparation techniques described by Plinius and Vitruvius; moreover it confirms the hypothesis that the artifacts are not fresco paintings. This work has been conducted within the context of a wider research on the Roman age mural paintings.
Forensic Science International
Journal of Forensic Science & Criminology, 2017
Observations by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) of un... more Observations by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) of unfired standard primer material (lead/antimony/barium) are presented from the centerfire cartridge primers of Winchester, Speer and Remington. Also examined by SEM/EDS are the surfaces of thirtytwo gunpowders (GPs) from Winchester, Federal, Hercules, DuPont and Remington. Compounds of sulfur, potassium and barium as well as primer-like particles composed of lead, antimony and barium were found on the surfaces of many of these GPs. The elements of these compounds likely contribute to gunshot residue (GSR) generated by the discharge of a firearm. We introduce the term, ―hybrid GSR‖ which will account for both the contribution to primer GSR by the interior firearm surfaces GSR and the elements associated with GP.
Egyptian Journal of Forensic Sciences 13 (2023), 2023
The forms and compositions of primer gunshot residue (GSR) in shooting cases have been routinely ... more The forms and compositions of primer gunshot residue (GSR) in shooting cases have been routinely analyzed in many crime labs by scanning electron microscope/energy-dispersive X-ray spectroscopy (SEM/EDS). Gunshot residue studies over the last 30 years have identified a contribution by residual GSR from surfaces within the firearm to GSR (the “memory effect”). In this study, we first focus on the GSR compositional differences between target, bore, and cylinder gap for a .22 caliber revolver which has received little attention in the literature. Secondly, we examine the behavior of elements involved in the residual contribution to GSR for a .22 caliber pistol.
Forensic Chemistry Available online 9 January 2023, 100472 In Press, Journal Pre-proofWhat are Jo... more Forensic Chemistry
Available online 9 January 2023, 100472
In Press, Journal Pre-proofWhat are Journal Pre-proof articles?
On the problem of data interpretation in the analysis of iron-containing GSR particles
Author links open overlay panelMarcoRomeoaFeliceNunziatae
https://doi.org/10.1016/j.forc.2023.100472
Get rights and content
Highlights
•
Iron is an element that can be present within a GSR particle;
•
The iron present in a GSR particle can be derived from several sources;
•
Forensic experts hypothesize that the iron may have come from the barrel of the firearm;
•
Several iron particles from the barrel of the firearm and other sources were analyzed;
•
In gunfire with rusty barrels, iron particles aggregate with GSRs in the cooling phase.
Abstract
Many forensic experts hypothesize that iron found in gunshot residues (GSRs) derive from melted iron particles because the steel of the barrel consists mainly of iron. This is a strong hypothesis that deserve careful investigation. To this purpose, we focused our attention on erosion and corrosion mechanism occurring in the barrel that can influence GSRs. A preliminary physicochemical interpretation consistent with the analytical results was presented. Moreover, spectra and images of GSRs originated from the firing of ammunition by firearms having rusty barrels and of iron oxide particles not originated from the firing were analyzed. The obtained results are discussed, taking into account the chemical content and morphology of the observed particles taking in account the context both of the erosion and of the corrosion and of the GSRs formation process
Inorganic gunshot residue (GSR) analysis is carried out by scanning electron microscopy/energy-di... more Inorganic gunshot residue (GSR) analysis is carried out by scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS)
in many forensic laboratories. Characteristic GSR often consists of lead–barium–antimony, commonly associated with sulfur. The strength
of forensic GSR evidence increases when unusual elements are found in residues collected both from the suspect and from the discharged
firearm. The presence of molybdenum in GSR, due to the use of MoS 2 lubricants in firearms, is experimentally demonstrated here for the
first time. The most intense molybdenum X-ray emissions are MoL peaks at 2.3 keV which overlap with PbM and SK families due to the
poor resolution of EDS detectors. When Pb, S, and Mo are allegedly present in the same particle, the reliability of automatic EDS routines is
at risk. Missing identifications or false detections and exclusions may then occur. Molybdenum should be considered as detected only if
MoK emissions meet the peak-to-background ratio minimum requirements. A strategy to spot Mo-containing residues is described,
based on the automated search of MoS 2 , using a new “Sulfur only” class added to the classification scheme, followed by careful manual
review of all GSR particles at an acceleration voltage of 30 kV. Our proposal improves commonly adopted forensic procedures currently
followed in casework.
The surfaces of thirty-one gunpowders (GPs) from Winchester, Federal, Hercules, DuPont, and Remin... more The surfaces of thirty-one gunpowders (GPs) from Winchester, Federal, Hercules,
DuPont, and Remington were examined by scanning electron microscopy/energy
dispersive X-ray spectroscopy. Particles and surface coatings on 22 of the GPs had
compositions of sulfur/potassium/barium or sulfur/potassium detected. Primer-like
particles composed of lead/antimony/barium were found on surfaces of twelve GPs.
Gunpowders from fifteen different lots of Winchester 9 mm Silvertip ® hollow point
cartridges were found to vary in GP type (flake and flattened ball) and associated
inorganic compounds of sulfur/potassium/barium or sulfur/potassium or one with
only potassium. No inorganic particles or coatings were detected on two of these
Winchester GPs. The elements from the inorganic compounds on GPs likely contrib-
ute to gunshot residue generated by the discharge of a firearm.
MERCURY STRUCTURAL SEGREGATION IN RESIDUE OF MERCURY FULMINATE IN RESIDUE OF MERCURY FULMINATE BASED PRIMERS BASED PRIMERS, 2019
In this work we propose the hypothesis that the chemical-physical properties of mercury can deter... more In this work we propose the hypothesis that the chemical-physical properties of mercury can determine its relative evanescence in GSR: in the other words we propose preliminary experimental results from which we derive, in according to thermodynamic laws, an possible explanation in term grain refinement, segregation and diffusion hybrid model.
Journal of Analytical Atomic Spectrometry, 2019
Standard analysis of inorganic gunshot residue aims nowadays at lead, antimony and barium particl... more Standard analysis of inorganic gunshot residue aims nowadays at lead, antimony and barium particles of spherical shape, although other elements are detected that may be indicative of the ammunition brand or interaction with specific materials. Calcium and phosphorus can be present in the particle systems examined. There are two main sources of these elements in gunshot residue: components of the ammunition, e.g. Eley brand .22 long rifle caliber and bone fragments created during contact and close-range shooting. Samples of human bones of various ages and the residue from the interior of spent cartridges of ten different products of Eley brand .22 long rifle caliber ammunition were systematically characterised as reference materials to aid the interpretation of candidate GSR particles detected in evidence samples. We found that Ca : P ratios obtained by means of scanning electron microscopy with energy dispersive X-ray spectrometry from GSR particles larger than about 10 micrometres characterised bone fragments reliably. Although Ca and P may be detected as traces, for smaller (micron and sub-micron) particles the Ca : P ratio is not a reliable indicator of bone material. But in such cases qualitative interpretation taking into account interdisciplinary information can be achieved for forensic purposes. Three case studies encompassing various types and amounts of gunshot residue identified the possibilities and limitations in the differentiation between the potential sources of calcium and phosphorus present in inorganic gunshot residue.
In their first full report on the analysis of GSR by SEM-EDS, Wolten and colleagues stated that t... more In their first full report on the analysis of GSR by SEM-EDS, Wolten and colleagues stated that the great majority of the gunshot residue particles (GSR), between 70 to 100%, have a characteristic morphology thus providing a detection criterion holding significance equal to that provided by the elemental composition. In fact, the particles must have a spherical or spheroidal shape and their surface should appear amorphous, devoid of any crystalline characteristic.
On a gunshot residue three-dimensional roundedness For the proper identification of GSR by SEM/ED... more On a gunshot residue three-dimensional roundedness
For the proper identification of GSR by SEM/EDX, together with a correct and congruent elemental analysis, is also essential to take into account the morphology of the particles and the nature of their surfaces. GSR corpuscles are formed during a rapid solidification process and, having assumed at the liquid state a spherical shape, they maintain this characteristic as solidification occurs. Their surfaces, probably due to a phenomenon of "grain refinement" , should appear completely amorphous at the normal working magnification with no trace of crystalline formations. This principle has been expressed already in 1977 by G.M. Wolten and colleagues in their fundamental work , and has been confirmed over the years by all the experienced scientists of the field including Prof. Carlo Torre and many others until Mar 2016.
Il libro espone tutto quanto è necessario sapere per progettare un poligono di tiro per ogni tipo... more Il libro espone tutto quanto è necessario sapere per progettare un poligono di tiro per ogni tipo di tiro; balistica, rimbalzo dei proiettili, acustica,inquinamento da piombo, pericolo di incendio ed esplosioni, normativa da applicare per licenze e gestione. In allegato le linee guida tedesche e canadesi e le circolari del Min. della Difesa. Riccamente illustrato.
NÉRON Librairie Arthème Fayard, Paris, 1962 Prima edizione italiana, tradotta a cura di ALESSAN... more NÉRON
Librairie Arthème Fayard, Paris, 1962
Prima edizione italiana, tradotta a cura di ALESSANDRO LESSONA E RICCARDO M. DEGLI UBERTI
Questa rassegna prende origine dalle problematiche relative all'arricchimento dell'uranio ai fini... more Questa rassegna prende origine dalle problematiche relative all'arricchimento dell'uranio ai fini della produzione di materiale fissile, segnatamente alle tecnologie ed ai processi industriali che ne determinano i sottoprodotti tra cui l'uranio impoverito, prosegue con la caratterizzazione di quest'ultimo, dei suoi impieghi bellici e della sua distribuzione nelle matrici biologiche ed ambientali. Nello specifico la tematica dell'arricchimento verrà trattata fornendo un taglio in termini di teoria fisica che partendo dai paradigmi interpretativi della meccanica statistica classica approfondirà gli aspetti isotopici alla luce della termodinamica, della fisica statistica e della meccanica quantistica.
Forensic Science International: Reports, 2022
Gelatina balistica: un approccio non newtoniano
Forensic Science Medicine and Pathology, 2023
Ballistic soap blocks are used in wound ballistics to assess the potential damage of the ammuniti... more Ballistic soap blocks are used in wound ballistics to assess the potential damage of the ammunition employed, allowing observation of the energy transfer occurred along the wound channel. The density and viscosity of ballistic soap (also called tissue simulant) simulate, to a good degree of approximation, the effect resulting from the interaction of penetrating bullets with living human soft tissue. Ballistic soap has a “plastic reaction” to bullet penetration, and therefore, unlike ballistic gelatin, the expansion of temporary cavity remains imprinted in the tissue simulant. When the soap blocks are sectioned or divided with nondestructive instrumental techniques (e.g., Compton’s scattering tomography), it’s possible, therefore, to observe the temporary cavity determined by the penetration of the bullet. This study provides insight into the severity of injuries originated from two different types of bullets of the same caliber by employing ballistic soap as a tissue simulant. In addition, it provides guidance to forensic practitioners on the proper use of ballistic soap for simulating gunshot wounds. The semi-computational approach employed, based on the results obtained from the firing tests, allowed the authors to understand that there is likely a threshold value of projectile energy density, close to 1 J/mm², beyond which its penetration into the ballistic soap ceases.