Accurate Isotopic Analysis Research Articles

A Simple Water Sample Storage Test for Water Isotope Analysis

Water is pivotal for human societies’ sustainability and resilience. Isotope hydrology and hydrogeology research plays an important role in understanding and managing water resources. Reliable scientific results hinge on high-quality data. Preventing water sample evaporation is essential for accurate isotopic analysis. In this study, the impacts on the quality of isotopic data were tested for the storage of water samples and the repetitive opening of a laboratory reference material (LRM) sub-sample replica during daily operation. Twenty 15 mL water samples were stored in high-density polyethylene (HDPE) bottles at room temperature and humidity to simulate storage conditions. One 60 mL water sample was collected from the same starting batch to simulate the LRM sub-sample. Each 15 mL sample was analysed once over 80 days for the isotopic composition of oxygen (δ18O) and hydrogen (δ2H). The 60 mL sample was repeatedly analysed in the same period. The data were tested to identify shifts in the isotopic composition induced by evaporative processes. The main results of the work are the following: (i) storage of the 15 mL water samples did not cause detectable evaporation in the testing period; (ii) the 60 mL δ18O values showed evidence of evaporation as proved by the positive shift of the isotopic data; (iii) the repetitive opening of the 60 mL sample was the main cause of evaporation; (iv) five openings can already cause detectable isotopic enrichment. Careful manipulation and frequent replacement of the LRM are thus necessary to prevent deterioration of the quality of the analyses.

Precise and accurate isotopic analysis of uranium and thorium in uranium ore concentrates using ICP-MS and their age dating for nuclear forensic analysis

Precise and accurate analysis of 235U/238U, 234U/238U, 230Th/234U and 230Th/232Th in 15 uranium ore concentrates (UOCs) was achieved using ICP-MS for nuclear forensic applications. A novel method was developed to dating UOCs.

Efficient preconcentration of ultra-trace rhenium from geological materials via induced adsorption for accurate isotope analysis

Preconcentration via induced adsorption achieves the quantitative recovery of Re and facilitates Re isotope analysis.

A new working reference material for cassiterite oxygen isotope microanalysis

Cassiterite is the principal ore mineral for tin, and its oxygen isotope is a promising proxy to trace the origin and evolution of ore‐forming fluids, which requires precise and accurate oxygen isotopic analysis. Secondary ion mass spectrometry (SIMS) is a powerful tool for oxygen isotope analysis, especially when samples bear complicated textures, but matrix‐matched reference materials are critical for accurate microanalysis. The only available matrix‐matched reference material for cassiterite oxygen isotope analysis is Yongde‐Cst, and more reference materials are required. Here, we report Piaotang‐Cst as a potential working reference material for cassiterite oxygen isotope microanalysis. Our extensive SIMS microanalysis confirmed that Piaotang‐Cst is relatively homogeneous, with an average two standard deviations (2SD) of 0.49‰ (n = 626). The δ18OVSMOW value of Piaotang‐Cst is 5.33 ± 0.07‰ (2SD, n = 5) as determined by a conventional fluorination isotope ratio mass spectrometer. We also demonstrated that there is no measurable matrix effect caused by the variable contents of trace elements for cassiterite oxygen isotope microanalysis. We proposed that the Piaotang‐Cst can be used as a working reference material for monitoring the external reproducibility and accuracy of SIMS analysis.

Analytical performance of single particle aerosol mass spectrometer for accurate sizing and isotopic analysis of individual particles

The commercial Hexin Single particle aerosol mass spectrometer (SPAMS) has been widely used for environmental aerosol monitoring and source apportionment. However, particle size measurement is easily affected by environment pressure fluctuation and sampling orifice clogging. The capability for quantitative analysis is poor, and few isotope measurement has been reported. This paper aims to evaluate the analytical performance of SPAMS and extend its application. First, the flight time of standard particles having different densities and sizes was measured under various conditions (aerodynamic lens upstream pressure and carrier gas). We proposed a universal method for particle size calibration, measurement and correction, taking into account the effects of lens geometry (acceleration nozzle diameter), particle parameters (density, diameter, and shape factor), and operating conditions (lens upstream pressure and carrier gas). Then, isotope measurement was performed when introducing a solution droplet containing a single element. Metal oxide and metal cluster ions were observed in the mass spectrum, indicating incomplete ionization of the sample droplet. The mass discrimination effect was carefully evaluated to correct the measured isotope ratio. Results show that the achievable accuracy of the corrected isotope ratio for elements investigated was 5%. The instrumental performance was relatively poor for elements having great ionization potential or bond energy. Finally, Ag/Eu2O3 suspension and yellow cake/ethanol suspension were analyzed for size, elemental and isotopic analysis. We confirmed that the mass discrimination effect during suspension introduction could be corrected using the mass discrimination correction factor obtained during solution introduction. The Ag, Eu and U in these suspension particles were all found to be at natural abundance. The uranium in the yellow cake was identified as sodium duranyate (Na2U2O7) with volumetric equivalent diameter of approximately 65 nm. The work presented here is beneficial for instrument improvement and wide application.

Safe, accurate, and precise sulfur isotope analyses of arsenides, sulfarsenides, and arsenic and mercury sulfides by conversion to barium sulfate before EA/IRMS

The stable isotope ratios of sulfur (δ34S relative to Vienna Cañon Diablo Troilite) in sulfates and sulfides determined by elemental analysis and isotope ratio mass spectrometry (EA/IRMS) have been proven to be a remarkable tool for studies of the (bio)geochemical sulfur cycles in modern and ancient environments. However, the use of EA/IRMS to measure δ34S in arsenides and sulfarsenides may not be straightforward. This difficulty can lead to potential health and environmental hazards in the workplace and analytical problems such as instrument contamination, memory effects, and a non-matrix-matched standardization of δ34S measurements with suitable reference materials. To overcome these practical and analytical challenges, we developed a procedure for sulfur isotope analysis of arsenides, which can also be safely used for EA/IRMS analysis of arsenic sulfides (i.e., realgar, orpiment, arsenopyrite, and arsenian pyrite), and mercury sulfides (cinnabar). The sulfur dioxide produced from off-line EA combustion was trapped in an aqueous barium chloride solution in a leak-free system and precipitated as barium sulfate after quantitative oxidation of hydrogen sulfite by hydrogen peroxide. The derived barium sulfate was analyzed by conventional EA/IRMS, which bracketed the δ34S values of the samples with three international sulfate reference materials. The protocol (BaSO4-EA/IRMS) was validated by analyses of reference materials and laboratory standards of sulfate and sulfides and achieved accuracy and precision comparable with those of direct EA/IRMS. The δ34S values determined by BaSO4-EA/IRMS in sulfides (arsenopyrite, arsenic, and mercury sulfides) samples from different origins were comparable to those obtained by EA/IRMS, and no sulfur isotope fractionations were introduced during sample preparation. We report the first sulfur isotope data of arsenides obtained by BaSO4-EA/IRMS.Graphical abstract

Non-matrix-matched calibration of Mg isotopic ratios in silicate samples by fs-LA-MC-ICP-MS with low mass resolution under wet plasma conditions

Accurate and precise Mg isotopic analysis by fs-LA-MC-ICP-MS can be performed with low mass resolution and non-matrix-matched calibration.

Accurate lithium isotopic analysis of twenty geological reference materials by multi-collector inductively coupled plasma mass spectrometry

The lithium (Li) isotopes can be used to track the evolution of continental silicate weathering, which has an important role in maintaining Earth's long-term climate stability. At present, complex separation procedures and analytical mass bias restrict the accurate determination of Li isotopic compositions in various geological samples with different Li concentrations and matrix/Li ratios. Here, an optimization of dual-column chromatography achieves high Li recovery, low procedural blank, and low Na/Li ratio (< 1) after purification, allowing the acquisition of high precision Li isotope ratios by a Nu Plasma 3 multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). In order to evaluate the accuracy of new method, the δ7Li values of BHVO-2, BCR-2, AGV-2, JG-2, RGM-2, SGR-1b, GSR-6, GSR-12, and seawater, are repeatedly analyzed more than 3 times each and are consistent with the published data within the uncertainty. The long-term external reproducibility of δ7Li based on L-SVEC and IRMM-016 pure solutions is about ±0.2‰ (2SD), and is suitable for analysis of geological samples. These results suggest that new dual-column method is reproducible and reliable. We also report ten new reference materials including two USGS rocks (SDC-1: 1.8 ± 0.4‰; W-2a: 2.9 ± 0.3‰), four soils (GSS-3: 1.3 ± 0.2‰; GSS-4: −5.1 ± 0.4‰; GSS-6: −1.9 ± 0.3‰; GSS-8: 0.4 ± 0.3‰), and four stream sediments (GSD-6: −1.0 ± 0.4‰; GSD-11: 1.1 ± 0.3‰; GSD-12: 1.8 ± 0.2‰; GSD-14: 1.6 ± 0.4‰), all previously analyzed for K isotopes. There is significantly fractionation of Li and K isotopes during silicate weathering. Compared to the K isotopes, Li isotopes have more promising as an isotope tool for weathering due to its larger fractionation and its abiotic property.

Direct Comb Vernier Spectroscopy for Fractional Isotopic Ratio Determinations.

Accurate isotopic composition analysis of the greenhouse-gasses emitted in the atmosphere is an important step to mitigate global climate warnings. Optical frequency comb–based spectroscopic techniques have shown ideal performance to accomplish the simultaneous monitoring of the different isotope substituted species of such gases. The capabilities of one such technique, namely, direct comb Vernier spectroscopy, to determine the fractional isotopic ratio composition are discussed. This technique combines interferometric filtering of the comb source in a Fabry–Perot that contains the sample gas, with a high resolution dispersion spectrometer to resolve the spectral content of each interacting frequency inside of the Fabry–Perot. Following this methodology, simultaneous spectra of ro-vibrational transitions of CO and CO molecules are recorded and analyzed with an accurate fitting procedure. Fractional isotopic ratio C/C at 3% of precision is measured for a sample of CO gas, showing the potentialities of the technique for all isotopic-related applications of this important pollutant.

Revisiting apatite SIMS oxygen isotope analysis and Qinghu-AP reference material

Oxygen is one of the most abundant elements in the universe and ubiquitously participates in geological and biological processes which play a critical role in shaping and maintaining habitability of the Earth. Its isotope composition is a key parameter to decode these geological and biological processes. For example, oxygen isotope composition of biogenic and abiogenic apatite are ideal proxies to reconstruct sea surface temperature and to tackle elemental cycling respectively, in which accurate and precise apatite oxygen isotope analysis is a basic requirement. Our robust evaluation demonstrates a lack of crystallographic orientation effects for Secondary Ion Mass Spectrometry (SIMS) apatite oxygen isotope analysis (expressed as δ18O). Apatite grains separated from the Qinghu monzonite were extensively analyzed by SIMS in the past decade in our laboratory, and 2041 individual δ18O measurements yield a two-standard-deviation of 0.47‰ (per mil, V-SMOW), or 0.16‰ when these measurements were integrated into 195 sessions. Homogenous oxygen isotope composition of Qinghu apatite (Qinghu-AP) at the micrometer level makes it a suitable reference material with a recommended δ18O value of 5.59 ± 0.19‰, as measured by Gas Source Isotope Ratio Mass Spectrometry with further validation from oxygen isotope thermometry. For seven randomly selected IGG (Institute of Geology and Geophysics)-Durango apatite crystals, our SIMS measurements suggest that they also have homogenous δ18O values (9.70 ± 0.22‰, 2 SD, n = 241, using Qinghu-AP as standard) without the presence of inter-grain and intra-grain heterogeneity. We documented a Y-coordinate related artificial effect, with measured δ18O values gradually increasing by ~1‰ from bottom to top of the mount over a distance of ~1.2 cm. This artifact is most likely caused by the presence of a slope (imperfect sample preparation and loading) or a gradient of accelerating voltage (conductivity of holder and sample) on the sample surface along the Y direction, which leads to an imperfect centering of the trajectory of the secondary ions. This effect can be reduced through applying a DTFA (dynamic transfer field aperture)-X correction. The presence of position-specific oxygen isotope fractionation could cause an artificial bias up to −6.7‰ when analyzing carbonated hydroxyapatite, and can reconcile the offset (e.g., −0.9 to 3.3‰) between δ18O values of conodonts measured by SIMS and IRMS. When working on hydrous systems (e.g., ore deposits) and low temperature environment (e.g., conodonts), where apatite is known to be water-rich and could be carbonated, a rigorous evaluation on this artificial bias is warranted. Since position-specific oxygen isotope fractionation is a common phenomenon observed in a variety of minerals (e.g., goethite, tourmaline and muscovite), attention should be paid in future studies. Our study highlights that SIMS is capable of providing accurate and precise δ18O measurements at the ~0.2‰ level, but high-quality reference materials and rigorous evaluations of potential artificial effects (e.g., topography, position, matrix, orientation, sample holder and position-specific oxygen isotope fractionation) degrading analytical accuracy are prerequisites.

Comprehensive analysis of laboratory boron contamination for boron isotope analyses of small carbonate samples

Boron isotopes are widely used as a proxy of marine carbonate in paleoclimatology to reconstruct seawater pH and atmospheric pCO2, and precise and accurate boron isotopic analysis is required for this purpose. Determination of boron isotopic composition is susceptible to contamination, especially for sample analyses with small amounts of boron; however, sources of experimental and laboratory contamination are not clearly evaluated. In this study, boron and boron isotope contamination during the analysis of small carbonate samples were examined in detail during sample cleaning, sample storage, chemical separation, and isotope measurement. Repeated cleaning of foraminifera shells using H2O with ultrasonication effectively minimized boron contamination from clay-rich material; however, an additional cleaning step with methanol and H2O2 is recommended to obtain repeatable precise δ11B, δ18O, and Mg/Ca values. Boron contamination during sample storage in a glass vial was far greater than expected. Glass-derived boron attached to foraminifera shells could not be completely removed by any physical or chemical cleaning process and influenced the δ11B value significantly. Even when a low-boron HEPA, boron-free HEPA, or ULPA filter was used for air-handling in the laboratory, airborne contamination by gaseous boron can still be significant, with seasonal variation in abundance and isotopic composition. Although this affects the procedural blank of boron during chemical separation, an acid-removing chemical filter can reduce the airborne boron flux. An autosampler in the MC-ICPMS analysis might be an additional source of airborne boron contamination.

Determination of Uranium Isotopic Ratio by ICP-OES Using Optimal Sensitivity Position Analysis.

Isotopic composition analysis of natural and depleted uranium by inductively coupled plasma optical emission spectrometry (ICP-OES) requires the use of a high-resolution instrument due to the very slight isotopic shifts between the atomic emission spectra of the 238U and 235U isotopes. In this work, we show that conventional ICP-OES (without high-resolution optics) can be used for highly accurate uranium isotopic analysis, on par with the results obtained by ICP-MS. Such accurate measurements are achieved by applying a preparatory mathematical procedure termed the optimal sensitivity position (OSP) procedure. In the OSP procedure, a theoretical spectrum for 238U is constructed and subtracted from the measured spectra of calibration solutions encompassing various isotopic ratios. The resultant spectra are used to locate the optimal measurement positions for both major uranium isotopes (238U and 235U) and the background measurement position. Herein, the optimal measurement positions are revealed to be located not at each isotope's peak maximum but at 424.427, 424.409, and 424.390 nm for 238U, 235U, and the background position, respectively. These locations remained stationary during the period of this work, implying that the use of a routine mathematical procedure is not required before every analysis. The OSP procedure offers a direct and highly accurate approach for determining the isotopic ratio of uranium in a relatively cheap and simple fashion. Furthermore, this work also demonstrates the possibility of greatly enhancing ICP-OES capabilities using mathematical analysis of spectra.

Chromatography purification of Rb for accurate isotopic analysis by MC-ICPMS: a comparison between AMP-PAN, cation-exchange, and Sr resins

Three methods were developed for purifying Rb from natural samples for isotopic analysis.

Atom Probe Mass Spectrometry of Uranium Isotopic Reference Materials.

Atom probe tomography (APT)-based isotopic analyses are becoming increasingly attractive for analysis applications requiring small volumes of material and sub-micrometer length scales, such as isotope geochemistry, nuclear safety, and materials science. However, there is an open question within the atom probe community as to the reliability of atom probe isotopic and elemental analyses. Using our proposed analysis guidelines, in conjunction with an empirical calibration curve and a machine learning-based adaptive peak fitting algorithm, we demonstrate accurate and repeatable uranium isotopic analyses, via atom probe mass spectrometry, on U3O8 isotopic reference materials. By using isotopic reference materials, each measured isotopic abundance value could be directly compared to a known certified reference value to permit a quantitative statement of accuracy. The isotopic abundance measurements for 235U and 238U in each individual APT sample were consistently within ±1.5% relative to the known reference values. The accuracy and repeatability are approaching values consistent with measurements limited primarily by Poisson counting statistics, i.e., the number of uranium atoms recorded.

N&amp;lt;sub&amp;gt;2&amp;lt;/sub&amp;gt;O isotopocule measurements using laser spectroscopy: analyzer characterization and intercomparison

Abstract. For the past two decades, the measurement of nitrous oxide (N2O) isotopocules – isotopically substituted molecules 14N15N16O, 15N14N16O and 14N14N18O of the main isotopic species 14N14N16O – has been a promising technique for understanding N2O production and consumption pathways. The coupling of non-cryogenic and tuneable light sources with different detection schemes, such as direct absorption quantum cascade laser absorption spectroscopy (QCLAS), cavity ring-down spectroscopy (CRDS) and off-axis integrated cavity output spectroscopy (OA-ICOS), has enabled the production of commercially available and field-deployable N2O isotopic analyzers. In contrast to traditional isotope-ratio mass spectrometry (IRMS), these instruments are inherently selective for position-specific 15N substitution and provide real-time data, with minimal or no sample pretreatment, which is highly attractive for process studies. Here, we compared the performance of N2O isotope laser spectrometers with the three most common detection schemes: OA-ICOS (N2OIA-30e-EP, ABB – Los Gatos Research Inc.), CRDS (G5131-i, Picarro Inc.) and QCLAS (dual QCLAS and preconcentration, trace gas extractor (TREX)-mini QCLAS, Aerodyne Research Inc.). For each instrument, the precision, drift and repeatability of N2O mole fraction [N2O] and isotope data were tested. The analyzers were then characterized for their dependence on [N2O], gas matrix composition (O2, Ar) and spectral interferences caused by H2O, CO2, CH4 and CO to develop analyzer-specific correction functions. Subsequently, a simulated two-end-member mixing experiment was used to compare the accuracy and repeatability of corrected and calibrated isotope measurements that could be acquired using the different laser spectrometers. Our results show that N2O isotope laser spectrometer performance is governed by an interplay between instrumental precision, drift, matrix effects and spectral interferences. To retrieve compatible and accurate results, it is necessary to include appropriate reference materials following the identical treatment (IT) principle during every measurement. Remaining differences between sample and reference gas compositions have to be corrected by applying analyzer-specific correction algorithms. These matrix and trace gas correction equations vary considerably according to N2O mole fraction, complicating the procedure further. Thus, researchers should strive to minimize differences in composition between sample and reference gases. In closing, we provide a calibration workflow to guide researchers in the operation of N2O isotope laser spectrometers in order to acquire accurate N2O isotope analyses. We anticipate that this workflow will assist in applications where matrix and trace gas compositions vary considerably (e.g., laboratory incubations, N2O liberated from wastewater or groundwater), as well as extend to future analyzer models and instruments focusing on isotopic species of other molecules.

Exploring the accuracy of isotopic analyses in atom probe mass spectrometry

Atom probe tomography (APT) can theoretically deliver accurate chemical and isotopic analyses at a high level of sensitivity, precision, and spatial resolution. However, empirical APT data often contain significant biases that lead to erroneous chemical concentration and isotopic abundance measurements. The present study explores the accuracy of quantitative isotopic analyses performed via atom probe mass spectrometry. A machine learning-based adaptive peak fitting algorithm was developed to provide a reproducible and mathematically defensible means to determine peak shapes and intensities in the mass spectrum for specific ion species. The isotopic abundance measurements made with the atom probe are compared directly with the known isotopic abundance values for each of the materials. Even in the presence of exceedingly high numbers of multi-hit detection events (up to 80%), and in the absence of any deadtime corrections, our approach produced isotopic abundance measurements having an accuracy consistent with values limited predominantly by counting statistics.

Chromatographic purification of antimony for accurate isotope analysis by MC-ICP-MS

A new purification approach is reported for the highly precise and accurate determination of Sb isotope ratios in geological samples.

Chlorine and bromine isotope fractionations of halogenated organic compounds in fragmentation by gas chromatography-electron ionization high resolution mass spectrometry

Revealing fractionations of chlorine and bromine isotope in electron ionization mass spectrometry (EI-MS) is crucial for accurate compound-specific isotope analysis of chlorine/bromine (CSIA-Cl/Br) for halogenated organic compounds (HOCs) using gas chromatography EI-MS (GC-EI-MS). This study investigated chlorine/bromine isotope fractionation of 12 organochlorines and 5 organobromines in EI-MS using gas chromatography-high resolution mass spectrometry. The observed isotope fractionations were evaluated with relative variation of chlorine/bromine isotope ratios (Δ37Cl or Δ81Br) between precursor ions and their product ions. All the 17 HOCs exhibited significant isotope fractionations with varied modes and magnitudes depending on compound and EI energy. The magnitudes of the observed isotope fractionations were extremely large in contrast to those in in-solution dehalogenation reactions, showing the Δ37Cl and Δ81Br values within the ranges of −149.2 to 292.0‰ and −362.2 to 546.2‰, respectively. Inter-ion and intra-ion isotope fractionations counteractively influenced the measured chlorine/bromine isotope ratios of individual dehalogenation product ions, whereas only the former could affect (enhance) the measured isotope ratios of molecular ions. The magnitudes of inter-ion isotope fractionation were generally lower than those of intra-ion isotope fractionation for most HOCs (11/17). Stable EI energy and isotope-ratio calculation using complete chlorine/bromine isotopologues of individual molecular ions help to obtain CSIA-Cl/Br data with high precision and accuracy. The results of this study could facilitate exploration of chlorine and bromine isotope fractionations of HOCs during dehalogenation in such conditions as photoinduced dehalogenation, and further elucidate relevant dehalogenation pathways in light of reaction mechanisms revealed by CSIA data.

In situ calcium isotopic ratio determination in calcium carbonate materials and calcium phosphate materials using laser ablation-multiple collector-inductively coupled plasma mass spectrometry

This study presents a highly precise and accurate Ca isotope analysis method using laser ablation multiple collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) in calcium carbonates and calcium phosphates. High-sensitivity cones and nitrogen gas were used to improve the performance of the LA-MC-ICP-MS. The experiment results show that at the N2 mode, the signal intensity of 44Ca+ in the high-sensitivity cones (Jet + X cones) was 5-fold higher than that in the normal cones (S + H cones), while the polyatomic interferences of 40Ar1H1H+ and 40Ar16O+ in the high-sensitivity cones were suppressed by factors of 6.1 and 10.6, respectively, after the addition of 8 ml min−1 N2. The combination of high sensitivity cones and N2 addition did not increase the production of double charged ions. Additionally, the interference correction of doubly charged Sr ions was investigated in detail. The experiment results demonstrate that the concentration ratio of Sr to Ca (represented as I87Sr++/I44Ca+), the 87Sr/86Sr ratio and the mass fractionation factor of Sr (fSr) during the measurement process were key parameters for in situ Ca isotope ratios analysis. The threshold values of these key parameters were evaluated and are recommended to ensure an accurate correction of doubly charged Sr ions. Using the optimized instrumental conditions and correction strategies, an excellent within-run precision (<0.06‰, 2SE) and external reproducibility (<0.15‰, 2SD) for the microanalysis of δ44/42Ca915b were obtained in natural calcium carbonates and calcium phosphates. These precisions are better than the values previously reported in the literature regarding using LA-MC-ICP-MS. Matrix effects were observed during the in situ Ca isotope analysis among calcium carbonates, hydroxy calcium phosphates and igneous apatites. Using the matrix-matching standards, accurate δ44/42Ca915b values in natural materials with various matrices were achieved, confirming the availability of the proposed method to resolve the spatial variation of δ44/42Ca in natural materials.

Revision of forensics-relevant nuclear data in Sb127 β decay

With a half-life of 3.85(5) d, the fission product $^{127}\mathrm{Sb}$ is potentially useful for the characterization of fallout debris that would be collected for forensic analysis following a hypothetical nuclear event. The $\ensuremath{\beta}$ decay of $^{127}\mathrm{Sb}$ has many characteristic $\ensuremath{\gamma}$-ray lines, however, the majority of decay strength is concentrated in the three strongest lines near 686, 473, and 784 keV, based on low-precision spectroscopic measurements from decades ago. In a new measurement of $^{127}\mathrm{Sb}\phantom{\rule{4pt}{0ex}}\ensuremath{\beta}$ decay, obtained from radiochemical separations of U photofission products, we show that the energies of the 686 and 784 lines are actually shifted lower by 0.8 and 1.1 keV, respectively. Such large discrepancies in the nuclear data inhibit accurate isotopic analyses and have important implications, for example, on the assessment of fission debris that might be collected in the days following a nuclear event. Therefore, a new evaluation of $^{127}\mathrm{Sb}\phantom{\rule{4pt}{0ex}}\ensuremath{\beta}$ decay and appropriate revisions to the various nuclear databases are warranted. This paper reports a new set of $\ensuremath{\gamma}$-ray energies and relative intensities corresponding to $^{127}\mathrm{Sb}$ decay.