Development of ammonium bifluoride fusion method for rapid dissolution of trinitite samples and analysis by ICP-MS

Hubley, Nickolas; Brown, John W. N.; Guthrie, John; Robertson, John; Brockman, John

doi:10.1007/s10967-015-4371-3

Cited by 19 publications

(6 citation statements)

References 6 publications

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“…In a wet chemical sample analysis approach, Zhang et al processed felsic mineral samples, using a sequence of ABF reaction at 230 o C in sealed PFA vials, followed by further closed vessel treatment with liquid nitric acid, evaporation, dissolution in an acid solution, addition of internal standard(s), and dilution for liquid-nebulization ICP-MS analysis. 13 Hubley et al followed a very similar procedure for the decomposition and dissolution of milled trinitite glass for liquid nebulization ICP-MS. 14 In our laboratory, we have confirmed that diverse materials such as glass, milled quartz, standard reference sediments, and uranium ore standards can be fully decomposed by similar methods; zircon is challenging. 15 When used for sample dissolution, additional steps using nitric acid follow the ABF method.…”

Section: Introductionmentioning

confidence: 61%

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Grate

González

O’Hara

et al. 2017

Analyst

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Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

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Section: Introductionmentioning

confidence: 61%

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Grate

González

O’Hara

et al. 2017

Analyst

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“…Final dilution is completed with 2% HNO3. [32]. Hubley et al also reports using a 1:1 ratio of concentrated HNO3 and concentrated HF (total volume of 2mL) in a pressure microwave vessel.…”

Section: A Dissolution and Laser Ablationmentioning

confidence: 99%

Modern Advancements in Post-Detonation Nuclear Forensic Analysis

Stratz¹,

Gill²,

Auxier³

et al. 2016

IJNS

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Deterring nuclear terrorism is a critical national asset to support the preclusion of non-state actors from initiating a nuclear attack on the United States. Successful attribution of a detonated nuclear weapon, which includes locating the source of the radiological materials used in the weapon, allows for timely responsive measures that prove essential in the period following a nuclear event. In conjunction with intelligence and law enforcement evidence, the technical nuclear forensics (TNF) post-detonation community supports this mission through the development and advancement of expertise to characterize weapon debris through a rapid, accurate, and detailed approach. Though the TNF field is young, numerous strides have been made in recent years toward a more robust characterization capability. This work presents modern advancements in post-detonation expertise over the last ten years and demonstrates the need for continued extensive research in this field.

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“…Zhang et al 15 demonstrated that ABF can be effectively used for digestion in open and closed vessel processes. ABF has already been applied to various refractory mineral bearing ores such as Nb–Ta rich (coltan) ores, 16 rutile, ilmenite, and perovskite Ti-rich minerals; 17 post-detonation nuclear forensic analysis; 18 trinitrite samples; 19 forensic nuclear debris; 20 zircon; 21 and scheelite. 22 However, ABF can only decompose silicate-bound tin 23 in geological rock samples, whereas mineral cassiterite remains unattacked by any acid or the combination of HF–HNO 3 /HCl–HClO 4 .…”

Section: Introductionmentioning

confidence: 99%

Novel and rapid NH₄HF₂ assisted KH₂PO₄ fusion of pegmatite ores bearing refractory minerals for multi-element determination by atomic spectrometry

Kumari,

Krishnakumar,

Thomas

et al. 2024

J. Anal. At. Spectrom.

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Development of ammonium bifluoride fusion method for rapid dissolution of trinitite samples and analysis by ICP-MS

Cited by 19 publications

References 6 publications

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Modern Advancements in Post-Detonation Nuclear Forensic Analysis

Novel and rapid NH₄HF₂ assisted KH₂PO₄ fusion of pegmatite ores bearing refractory minerals for multi-element determination by atomic spectrometry

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Development of ammonium bifluoride fusion method for rapid dissolution of trinitite samples and analysis by ICP-MS

Cited by 19 publications

References 6 publications

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Modern Advancements in Post-Detonation Nuclear Forensic Analysis

Novel and rapid NH4HF2 assisted KH2PO4 fusion of pegmatite ores bearing refractory minerals for multi-element determination by atomic spectrometry

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Novel and rapid NH₄HF₂ assisted KH₂PO₄ fusion of pegmatite ores bearing refractory minerals for multi-element determination by atomic spectrometry