Rapid, molecule-free, in situ rare earth element abundances by SIMS-SSAMS

Groopman, Evan; Grabowski, K. S.; Fahey, A. J.; Kööp, L.

doi:10.1039/c7ja00294g

Cited by 8 publications

(16 citation statements)

References 45 publications

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“…Exponential fits to the molecular transmissions are also shown. As discussed in Groopman et al6 , the molecular dissociation cross sections appear to approximately scale with bond dissociation energy (e.g., Ta-O = 839 kJ/mol; La-O = 798; U-O = 758; Ti-O = 666; Si-Si = 310;…”

mentioning

confidence: 90%

“…On the SSAMS, the range of the switching is limited to the flight tube bias relative to the ion energy: ±20 kV / 304.5 kV ≈ ±6.5%. The gap lenses and flight tube act as an Einzel lens of non-ideal geometry, which affects the focal properties of the beam 6 . Within the ±6.5% switching range these effects are minor and we do not observe any fractionation.…”

Section: Nautilus Overviewmentioning

confidence: 99%

“…Dual Electrostatic Peak Switching Electrostatic peak switching on both SIMS and SSAMS simplifies synchronization of the two magnets in the NAUTILUS' MS-MS configuration. As described in Groopman et al 6 , the duty cycle of the instrument is improved due to more rapid switching times across the ±6.5% EPS range. A significant benefit is that masses may be analyzed in any order for a given magnetic field setting since EPS does not affect magnet hysteresis.…”

Section: Direct Molecule-free Raster Ion Imagingmentioning

confidence: 99%

“…Therefore, for analyses such as U-Th-Pb dating, when the magnet is tuned near the Pb isotopes, 206 Pb + or 208 Pb + may be measured and centered upon first before measuring the usually underabundant 204 Pb + peak. The magnet flight tube, when biased, acts as a lens, with different focal properties for accel-decel and decel-accel modes 6 . The SIMS spectrometer lens was calibrated to compensate for this effect automatically through the use of a gain factor when switching the EPS.…”

Section: Direct Molecule-free Raster Ion Imagingmentioning

confidence: 99%

“…PTFE sheets and tape were used to insulate the flight tube from the pole pieces and Hall probe. A schematic of the PEEK insulator with dimensions can be found in Groopman et al 6 .…”

Section: Electrostatic Peak Switching (Eps)mentioning

confidence: 99%

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An overview of NRL's NAUTILUS: a combination SIMS-AMS for spatially resolved trace isotope analysis

Groopman

Willingham

Fahey

et al. 2020

J. Anal. At. Spectrom.

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We present a description of the capabilities and performance of the NAval Ultra-Trace Isotope Laboratory's Universal Spectrometer (NAUTILUS) at the U.S. Naval Research Laboratory. The NAUTILUS combines secondary ion mass spectrometry (SIMS) and single-stage accelerator mass spectrometry (SSAMS) into a single unified instrument for spatially resolved trace element and isotope analysis. The NAUTILUS instrument is essentially a fully functional SIMS instrument with an additional molecule-filtering detector, the SSAMS. The combination of these two techniques mitigates the drawbacks of each and enables new measurement paradigms for SIMS-like microanalysis. Highlighted capabilities include molecule-free raster ion imaging for direct spatially resolved analysis of heterogeneous materials with or without perturbed isotopic compositions. The NAUTILUS' sensitivity to trace elements is at least 10× better than commercial SIMS instruments due to near-zero background conditions. We describe the design and construction of the NAUTILUS, and its performance applied to topics in nuclear materials analysis, cosmochemistry, and geochemistry. IntroductionAccelerator mass spectrometry (AMS) is synonymous with ultra-trace isotope analysis, while secondary ion mass spectrometry (SIMS) is the premier spatially resolved, sensitive, surface analysis technique. We have successfully designed and built the NAval Ultra-Trace Isotope Laboratory's Universal Spectrometer (NAUTILUS) at the U.S. Naval Research Laboratory (NRL) 4-9 , which combines the modified hardware from two commercial instruments, an Ametek Cameca ims 4f SIMS 10 and a National Electrostatics Corporation (NEC) single-stage AMS (SSAMS) 11-13 , together with custom control hardware and software. The motivation for this novel combination MS-MS instrument is to utilize the aforementioned advantages of each technique in a manner which simultaneously mitigates each technique's drawbacks. While SIMS maintains excellent sensitivity for materials analysis with down to micrometer spatial and nanometer depth resolution, the sputtering process produces molecular secondary ions. These may interfere at the same mass-tocharge ratio (m/z) with isotopes of interest, especially for high-mass and/or trace analyses. The trade-off between increased mass resolving power (MRP), typically defined as the full width at 10% peak height, and decreased instrumental transmission can make high-mass analyses impractical, especially for trace isotopes (e.g., detection of 236 U in the presence of 235 U 1 H) 14 . AMS excels at removing molecular isobaric interferences, but these instruments typically analyze bulk samples without spatial resolution either due to chemical sample preparation or large sputter source size. While SIMS may analyze positive or negative secondary ions, tandem AMS instruments are limited to injecting negative ions. This dramatically decreases their sensitivity to electropositive elements, since molecular ions such as FeOor UOmust be generated to transport the element of interest, Fe or U,...

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mentioning

confidence: 90%

Section: Nautilus Overviewmentioning

confidence: 99%

Section: Direct Molecule-free Raster Ion Imagingmentioning

confidence: 99%

Section: Direct Molecule-free Raster Ion Imagingmentioning

confidence: 99%

“…PTFE sheets and tape were used to insulate the flight tube from the pole pieces and Hall probe. A schematic of the PEEK insulator with dimensions can be found in Groopman et al 6 .…”

Section: Electrostatic Peak Switching (Eps)mentioning

confidence: 99%

See 3 more Smart Citations

An overview of NRL's NAUTILUS: a combination SIMS-AMS for spatially resolved trace isotope analysis

Groopman

Willingham

Fahey

et al. 2020

J. Anal. At. Spectrom.

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Instruments for Observations of Radioactivities

Kanbach¹,

Nittler²

2018

Astrophysics With Radioactive Isotopes

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Avoiding polyatomic interferences in measurements of lanthanides in uranium material for nuclear forensic purposes

Vesterlund

Ramebäck

2019

J Radioanal Nucl Chem

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Measurements of the lanthanide series with ICP-SF-MS provide low detection limits but suffer from oxides of the lighter lanthanides interfering on the heavier ones. In this work, two different methods to measure the lanthanide series without interferences, were investigated and compared to measuring the lanthanides directly with a standard sample introduction system. It is shown that by using a desolvating sample introduction system during measurements, the impact of polyatomic interferences are eliminated. It is also shown that using chemical separations to separate the elements in the lanthanide series into three fractions almost eliminates polyatomic interferences, while direct measurements with a standard sample introduction system may lead to inaccurate results due to interferences.Publisher's Note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

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Rapid, molecule-free, in situ rare earth element abundances by SIMS-SSAMS

Abstract: We present a novel method for rapid and high-sensitivity in situ measurements of the rare earth elements (REEs) by combined secondary ion mass spectrometry and single-stage accelerator mass spectrometry (SIMS-SSAMS).

Cited by 8 publications

References 45 publications

An overview of NRL's NAUTILUS: a combination SIMS-AMS for spatially resolved trace isotope analysis

An overview of NRL's NAUTILUS: a combination SIMS-AMS for spatially resolved trace isotope analysis

Instruments for Observations of Radioactivities

Avoiding polyatomic interferences in measurements of lanthanides in uranium material for nuclear forensic purposes

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