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Rapid Analysis of Trinitite with Nuclear Forensic Applications for Post-Detonation Material Analyses

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Rapid Analysis of Trinitite with Nuclear Forensic Applications for Post-Detonation Material Analyses 1 Rapid Analysis of Trinitite with Nuclear Forensic Applications for 2 Post-Detonation Material Analyses 3 4 Nicholas Sharp a*, William F. McDonougha, b*, Brian W. Ticknorc, Richard D. Ashb, Philip M. 5 Piccolib, Dana T. Borgb 6 7 aDepartment of Chemistry & Biochemistry 8 University of Maryland 9 College Park, MD 20742 10 USA 11 12 bDepartment of Geology 13 University of Maryland 14 College Park, MD 20742 15 USA 16 17 cChemical Sciences Division 18 Oak Ridge National Laboratory 19 1 Bethel Valley Road, MS 6415 20 Oak Ridge TN 37830 21 USA 22 23 24 *Corresponding authors: 25 Nicholas Sharp 26 Department of Chemistry & Biochemistry 27 University of Maryland 28 College Park, MD 20742 29 USA 30 Tel: (301)405-1830 31 Fax: (301)405-3597 32 [email protected] 33 34 William F. McDonough 35 Department of Geology 36 University of Maryland 37 College Park, MD 20742 38 USA 39 Tel: (301) 405-5561 40 Fax: (301) 405-3597 41 [email protected] 42 43 Keywords: Trinitite * Nuclear Forensics * Laser-ablation and solution inductively coupled mass 44 spectrometry * Nd and Gd isotopic ratios 45 Page 1 of 34 46 Abstract 47 Analysis of post-nuclear detonation materials provides information on the type of device 48 and its origin. Compositional analysis of trinitite glass, fused silicate material produced from the 49 above ground plasma during the detonation of the Trinity nuclear bomb, reveals gross scale 50 chemical and isotopic heterogeneities indicative of limited convective re-homogenization during 51 accumulation into a melt pool at ground zero. Regions rich in weapons grade Pu have also been 52 identified on the surface of the trinitite sample. The absolute and relative abundances of the 53 lanthanoids in the glass are comparable to that of average upper crust composition, whereas the 54 isotopic abundances of key lanthanoids are distinctly non-normal. The trinitite glass has a non- 55 normal Nd isotope composition, with deviations of -1.66 ± 0.48 ε (differences in parts in 104) in 56 142Nd/144Nd, +2.24 ± 0.32 in 145Nd/144Nd, and +1.00 ± 0.66 ε in 148Nd/144Nd (all errors cited at 57 2σ) relative to reference materials: BHVO-2 and Nd-Ames metal. Greater isotopic deviations 58 are found in Gd, with enrichments of +4.28 ± 0.72 in 155Gd/160Gd, +4.19 ± 0.56 in 59 156Gd/160Gd, and +3.59 ± 0.37 in 158Gd/160Gd compared to BHVO-2. The isotopic deviations 60 are consistent with a 239Pu based fission device with additional 235U fission contribution and a 61 thermal neutron fluence between 0.97 and 1.4 x 1015 neutrons/cm2. 62 Page 2 of 34 63 Introduction 64 Today, a well-documented chemical and isotopic database is needed to assign origin and 65 provenance to materials from a nuclear event. Characterizing the fissile material and 66 composition of an unknown device are central efforts of nuclear forensics which can be 67 challenging in the case of an urban event, given the myriad of debris types possible from the 68 local environment. In the case of a nuclear device, non-natural isotopic fingerprints have the 69 potential to provide insights into the history, source, and origin of interdicted materials. It is 70 critical to observe and understand the effects of a fission event on less-complicated material 71 before embarking on analyzing complex urban debris. Analyses of trinitite, fused silica-glass 72 from the Trinity test event, presents nuclear forensic investigators with ideal post-detonation 73 material where the composition of the nuclear device and source material are well-known, 74 enabling validation of testing methods designed to determine a device’s original makeup. In this 75 study, we present chemical and isotopic data on trinitite and compare our results with Trinity’s 76 known characteristics. 77 In the early hours of 16 July 1945 the atomic age began with the Trinity nuclear bomb 78 detonation at the White Sands Proving Ground, New Mexico. The bomb, a 239Pu implosion 79 device, produced a fireball of 104 K and a debris cloud that reached a height of 11 km within 80 minutes, and eventually as high as 21 km [1]. The debris cloud, consisting of material from the 81 detonation tower, the bomb itself, and adjacent desert sand, precipitated onto the desert floor and 82 cooled rapidly, yielding a glassy surface, trinitite, that surrounded the explosion site. 83 The four varieties of trinitite include: green glass trinitite, pancake trinitite, red trinitite, and 84 bead trinitite. All types originate from arkosic sand and are composed of quartz, microcline, 85 albite, muscovite, actinolite, and calcite [1]. The green glass variety (analyzed in this study) Page 3 of 34 86 consists of glass with no observable unaltered original sand material. This sample was likely 87 produced from the combination of proximal sand near ground zero melting into a glass and 88 falling material from the debris cloud [2]. However, due to remediation of the test site, the exact 89 location relative to ground-zero for this trinitite sample is unknown. 90 Trinitite contains fissile materials, neutron activated materials, and pieces of the detonation 91 tower and the bomb itself, such as the uranium tamper and lead casing [2-4]. Recently uranium 92 and lead isotopic signatures of the bomb have been investigated [5, 6]. Here we report on the 93 chemical and isotopic composition of trinitite, both spatially resolved laser ablation and solution 94 analyses, using inductively coupled plasma mass spectrometry. During detonation, fission 95 products of both light and heavy isotopes (e.g., 80-105 amu and 130-160 amu, respectively) are 96 produced. The tail of the heavy isotope product distribution includes the middle members of the 97 lanthanoids. The relative isotopic abundances of lanthanoids produced via fission differ from 98 those occurring naturally. The mixing of fission lanthanoids with natural material produces 99 measurable enrichments and depletions in isotopic abundances when compared to natural 100 material. The resultant altered isotopic abundances can be used to identify the device’s fissile 101 material, given a successful deconvolution of the fissile and natural isotopic compositions. 102 In this study the concentration of major element oxides and lanthanoids were determined 103 using a combination of electron probe micro-analysis (EPMA) and laser-ablation inductively- 104 coupled mass spectrometry (LA-ICP-MS). The isotopic composition of Gd and Nd were 105 determined by sample dissolution followed by chromatographic separation of the elements of 106 interest using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The 107 utility of rapid analysis of a post-detonation material via EPMA and LA-ICP-MS provides an Page 4 of 34 108 initial qualitative screening that readily identifies specific targets for more thorough analyses, in 109 this case using MC-ICP-MS for high-precision isotopic ratio determinations. 110 111 Experimental methods 112 113 The trinitite sample studied is entirely glass and contains little to no original sand. The green 114 glass has a smooth top which corresponds to the surface facing the atmosphere during 115 deposition. Deeper into the sample are vesicles with increasing frequency with greater depth. 116 Samples are highly heterogeneous in composition with vesicles accounting for approximately 117 33% of the total trinitite volume [7]. A ~1 g piece was broken off of the bulk pool glass and 118 subsequently split into two fractions by hand. Both were mounted in epoxy: one piece was 119 mounted with the smooth surface exposed; the other piece was mounted perpendicular to the 120 smooth surface (cross section; Fig 1). 121 122 Electron microprobe 123 124 The JXA-8900 SuperProbe was used to determine major element concentrations via 125 wavelength dispersive spectrometry (WDS). The analyses were carried out with a 10-20 μm spot 126 size, accelerating voltage of 15 kV, and a 20 nA cup current. Data was recalculated using a ZAF 127 algorithm using orthoclase (K2O, Al2O3, SiO2), rhodonite (MnO), and kakanui hornblende (CaO, 128 MgO, FeO, TiO2) as primary standards with Yellowstone rhyolite as a secondary standard. 129 Backscattered electron (BSE) images were also acquired. 130 Page 5 of 34 131 Sample digestion and chromatography 132 133 For Nd and Gd isotope analysis a 0.1 g piece of trinitite underwent an acid digestion 134 procedure consisting of a mixture of concentrated HNO3 and HF in addition to 100 µL of HClO4 135 in a sealed 15 mL Teflon beaker. Two 0.05 g BHVO-2 SRMs underwent the same procedure in 136 separate beakers. An analytical blank was also prepared and treated with the same chemistry 137 procedure and resulted in Nd and Gd blank concentrations of 6 pg. Teflon distilled acid was 138 used for sample digesting, chromatography, and sample analysis. 139 Sample digestion was performed on a hotplate set to 180°C for 72 hours. Subsequently 140 the beakers were opened and the solutions were dried to a hard residual cake; 6 M HCl was 141 added to each beaker, and they were then resealed and heated for an additional 24 hours. 142 Following this heating, the beakers were opened and allowed to dry again, and the 6M HCl step 143 was repeated. After the 3rd drying step 2 mL of quartz distilled 2.5 M HCl was added to the 144 samples. 145 Lanthanoids were separated from the bulk matrix with a 12cm x 2cm Dowex AG50W x8 146 400 mesh cation exchange column in H+ form. The 2 mL solution of 2.5 M HCl was added to 147 the column and 50 mL of 2.5 M HCl wash was added and followed by 45 mL of 4.5 M HNO3, 148 with the last 35 mL collected as the REE cut.
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