ABSTRACTRationaleInductively coupled plasma (ICP) is a commonly used ion source for mass spectrometry‐based chemical analysis of a wide range of materials. Traditional ICP ion sources use high power (> 1000 W) and significant gas flow (> 10 L/min), rendering them unsuitable for spaceflight, as they are too resource‐intensive for planetary spacecraft.MethodsTo address the technology gap, we designed and developed a laser ablation microwave‐induced plasma mass spectrometer (LA‐MIP‐MS) and experimentally validated the analytical performance of a prototype instrument capable of providing in situ analyses during planetary science missions. We developed a low‐pressure plasma ion source and interfaced it to a heritage quadrupole mass spectrometer (QMS) to perform elemental and isotopic analysis of solid samples via laser ablation. The low power plasma ion source was generated at < 1 Torr (< 133 Pa) using 30 W of power and 50 mL/min of He. Analytes were introduced via laser ablation (266 nm); we report elemental abundances and isotopic ratios for Cu, Ni, and Fe metals.ResultsOur experiments confirmed quantification accuracy for stainless steel within 1.4–4% of values measured by x‐ray fluorescence (XRF), with precision ranging from ±9.1 to 22% (2σm). Cu and Ni isotopic ratios were measured with ±0.8–3% (2σm) precision and reproducibility ranging from 0.12% to 11.8%. Measured limits of detection ranged from 21 ppmw for 57Fe to 780 ppmw for 54Fe, with limits of detection for Cr, Mn, and Ni below 240 ppmw.ConclusionsThis technique adds to the roster of instrumentation available for planetary missions by enabling elemental and isotopic analysis with orders of magnitude less power and plasma gas relative to commercial ICP‐MS systems. This work paves the way for low resource LA‐MIP‐MS instruments as a viable technique to be applied to a wide range of applications for terrestrial and spaceflight chemical analysis of geologic materials.

ABSTRACTRationaleReproducible analytical instrumentation system performance is critical for mass spectrometry, particularly metabolomics, aptly named system suitability testing. We identified a need based on literature reports that stated only 2% of papers performed system suitability testing.MethodsWe report MassQLab, built upon open‐source, vendor‐agnostic software called the mass spectrometry query language (MassQL). MassQL, implemented in MassQLab, provides freedom for researchers to choose their analyte/s, mass spectrometry system (including liquid chromatography—mass spectrometry), and metrics of performance.ResultsIn this report, we describe the use of MassQLab, demonstrate the construction of the required MassQL query, common metrics of performance (i.e., extracted ion chromatograms), uncommon metrics (i.e., MS/MS product ion spectra), and discuss insights gained about performance—including issues requiring correction prior to sample analysis.ConclusionsMassQLab is a flexible solution for system suitability testing for mass spectrometry‐based analytical measurements. Deficits in analytical performance, while unavoidable and rare, were noted prior to data collection and corrected. The open‐source and adaptable nature of MassQLab will empower researchers and lead to improved implementation of system suitability testing.

ABSTRACT The infrared multiphoton dissociation spectrum of the gas‐phase uranyl perchlorate anion ([UO 2 (ClO 4 ) 3 ] − ) was measured. The asymmetric uranyl stretch lies somewhere between 930 and 1030 cm −1 , though it could not be deconvoluted from a closely located perchlorate stretching mode. The experimentally measured spectrum was in good agreement with spectra calculated using density functional theory with the B3LYP and TPSSh functionals and Grimme's D3 dispersion corrections with Becke–Johnson damping. The calculations suggest that the asymmetric uranyl stretch lies in the range of 970–980 cm −1 , about 20–30 cm −1 higher than for the analogous uranyl trinitrato complex and consistent with perchlorate as a weaker ligand than nitrate. Like the uranyl trinitrato anion, fragmentation of [UO 2 (ClO 4 ) 3 ] − by collision‐induced dissociation resulted in loss of a ClO 3 • radical to form [UO 3 (ClO 4 ) 2 ] − . Infrared multiphoton dissociation measurements of [UO 3 (ClO 4 ) 2 ] − indicate that the structure of the product ion has an O − ligand bound to the uranyl in a T‐arrangement and two perchlorate ligands, matching the findings from uranyl nitrato complexes. The uranyl stretch in this complex was slightly separated from the perchlorate modes and was measured at 906 cm −1 , slightly higher than for the analogous nitrate complex, again consistent with perchlorate as a weaker ligand than nitrate in the gas phase.

ABSTRACTThe participants of the 12th International Atomic Energy Agency (IAEA) meeting on stable isotope reference materials reached a consensus, acknowledging the existence and use of two carbon isotope delta scales: the VPDB (Vienna Peedee belemnite) scale and the VPDB‐LSVEC (LSVEC ‐ lithium carbonate prepared by H. J. Svec). Conversion models between the two scales can be established and used but introduce uncertainty. A format for isotope delta scale definition was agreed upon and was used to define the two carbon isotope delta scales and the two main oxygen isotope delta scales, VSMOW‐SLAP (Vienna Standard Mean Ocean Water–Standard Light Antarctic Precipitation) and VPDB. Confirmation or identification of a second‐scale–defining point is still necessary for the nitrogen and sulfur isotope delta scales.Efforts are encouraged to improve consistency among laboratories in the isotopic analysis of “non‐exchangeable hydrogen” in bulk organic materials and oxygen in carbonates using the phosphoric acid reaction. Additional topics discussed include (1) need for improvement in reference materials for accurate greenhouse gas isotopic analyses; (2) reference materials under production by the IAEA, the US Geological Survey (USGS), and the US National Institute of Standards and Technology (NIST); (3) methods for value and uncertainty assignment of reference materials; and (4) calculation of carbon‐13 isotope delta and oxygen‐18 isotope delta of CO2 measured by dual‐inlet isotope ratio mass spectrometry.