Method For Isotopic Analysis Research Articles

Rapid, sensitive analysis method for determining the nitrogen stable isotope ratio of total free amino acids in soil.

The amino acid-nitrogen (AA-N) isotope analysis of naturally abundant or isotope-labeled samples is indispensable for tracing nitrogen transfer in soil nitrogen biogeochemical cycling processes. Despite the usefulness of AA-N isotope analysis, the preparation methods are complex and time-consuming, and necessitate the use of toxic reagents. We present an improved, rapid method for AA-N isotope analysis with high precision. At a high pH, AA-N was released and oxidized to N2 O using ClO- under vacuum. Additionally, purge-and-trap isotope ratio mass spectrometry was used to analyze N2 O. Moreover, we investigated the effect of various factors on the N2 O conversion process with glycine and applied the results to seven representative single-N AAs (alanine, serine, cysteine, aspartic acid, glutamic acid, leucine, and phenylalanine) and five poly-N AAs (lysine, arginine, histidine, tryptophan, and asparagine), as well as side-chain analogs, blank reagent, and other N forms. The concentration of ClO- and the pH were determined to be crucial factors for achieving desirable AA-N to N2 O conversion efficiencies. Glycine-N had the highest N2 O yield of 70%, with isotopic results consistent with those of the reference values at a high precision (within 0.5‰ for natural abundance and 0.01 atom% for 15 N-enrichment) at the nanomolar N level. Additionally, the α-NH2 AAs were labile, and the single-N AAs were more easily converted to N2 O than poly-N AAs. With the exception of γ-aminobutyric acid, the N2 O conversion efficiencies of the side-chain N analogs were very low (below 5%). This method was also applicable to the 15 N analysis of the total free AAs in complex soil samples without interference from analytical blanks and other forms of N. Our method is highly selective for the α-NH2 groups of an amino acid, and the oxidation of the side chain is difficult. In addition, the method is sensitive, rapid, and convenient, and does not require toxic reagents.

A rapid high‐precision analytical method for triple oxygen isotope analysis of CO2 gas using tunable infrared laser direct absorption spectroscopy

RationaleThe simultaneous analysis of the three stable isotopes of oxygen—triple oxygen isotope analysis—has become an important analytical technique in natural sciences. Determination of the abundance of the rare 17O isotope in CO2 gas using magnetic sector isotope ratio mass spectrometry is complicated by the isobaric interference of 17O by 13C (13C16O16O and 12C16O17O, both have mass 45 amu). A number of analytical techniques have been used to measure the 17O/16O ratio of CO2 gas. They either are time consuming and technically challenging or have limited precision. A rapid and precise alternative to the available analytical methods is desirable.MethodsWe present the results of triple oxygen isotope analyses using an Aerodyne tunable infrared laser direct absorption spectroscopy (TILDAS) CO2 analyzer configured for 16O, 17O, and 18O combined with a custom gas inlet system. We evaluate the sensitivity of our results to a number of parameters. CO2 samples with a wide range of δ18O values (from −9.28‰ to 39.56‰) were measured and compared to results using the well‐established fluorination‐gas source mass spectrometry method.ResultsThe TILDAS system has a precision (standard error, 2σ) of better than ±0.03‰ for δ18O and ±10 per meg for Δ′17O values, equivalent to the precision of previous analytical methods. Samples as small as 3 μmol CO2 (equivalent to 300 μg CaCO3) can be analyzed with a total analysis time of ~30 min.ConclusionsWe have successfully developed an analytical technique for the simultaneous determination of the δ17O and δ18O values of CO2 gas. The precision is equal to or better than that of existing techniques, with no additional chemical treatments required. Analysis time is rapid, and the system is easily automated so that large numbers of samples can be analyzed with minimal effort.

Fast and Efficient Atmospheric NO2 Collection for Isotopic Analysis by a 3D-Printed Denuder System.

Being major species of atmospheric reactive nitrogen, nitrogen oxides (NOx = NO + NO2) have important implications for ozone and OH radical formation in addition to nitrogen cycles. Stable nitrogen isotopes (δ15N) of NOx have been sought to track NOx emissions and NOx chemical reactivities in the atmosphere. The current atmospheric NOx collection methods for isotopic analysis, however, largely suffer from unverified collection efficiency and/or low collection speed (<10 L/min). The latter makes it difficult to study δ15N(NOx) in pristine regions with low NOx concentrations. Here, we present a three-dimensional (3D)-printed honeycomb denuder (3DP-HCD) system, which can effectively collect atmospheric NO2 (a major part of NOx) under a variety of laboratory and field conditions. With a coating solution consisting of 10% potassium hydroxide (KOH) and 25% guaiacol in methanol, the denuder system can collect NO2 with nearly 100% efficiency at flow rates of up to 70 L/min, which is 7 times higher than that of the existing method and allows high-resolution (e.g., diurnal or finer resolution) NO2 collection even in pristine sites. Besides, the δ15N of NO2 collected by the 3DP-HCD system shows good reproducibility and consistency with the previously tested method. Preliminary results of online NO oxidation by a chrome trioxide (CrO3) oxidizer for simultaneous NO and NO2 collection are also presented and discussed.

Stable carbon and hydrogen isotope fractionation of volatile organic compounds caused by vapor-liquid equilibrium

Several types of laboratory experiments were conducted to evaluate isotope fractionation caused by phase transfer process for a selection of common environmental contaminants. Carbon and hydrogen isotope fractionation caused by vaporization of non-aqueous phase liquid (NAPL), by volatilization from water and by dissolution into an organic solvent (tetraethylene glycol dimethylether or TGDE) under equilibrium conditions was investigated with closed system experimental setups to isolate the air-liquid partitioning process. A selection of aromatic, aliphatic and chlorinated compounds along with one fuel oxygenate (methyl tert-butyl ether or MTBE) were evaluated to determine isotope enrichment factor related to respective phase transfer process. During NAPL vaporization, the residual mass of aromatic compounds, aliphatic compounds and MTBE became progressively depleted in heavy carbon and hydrogen isotopes. In contrast, during volatilization from water, the residual mass of aromatic compounds and MTBE dissolved in the water became progressively enriched in heavy hydrogen isotopes, whereas no significant change in carbon isotope was observed, except for MTBE showing a significant depletion. For the air-TGDE partitioning process, most of the aromatic compounds tested led to no significant carbon (except ethylbenzene) or hydrogen (except toluene and o-xylene) isotope fractionation. In contrast, significant carbon isotope fractionation was observed for aliphatic and chlorinated compounds and hydrogen isotope fractionation for aliphatic compounds, and are comparable to progressive NAPL vaporization in direction and magnitude. The isotope fractionation factors determined in this study are key for interpreting the change in isotope ratios when assessing the fate of gas-phase VOCs present in the soil air or when gas-phase VOCs are sampled using TGDE as the sink matrix. The results of this study contribute to expand the list of common environmental contaminants that can be assessed by the compound-specific isotope analysis (CSIA) method deployed in the frame of gas-phase studies.

Dietary niche separation of three Late Pleistocene bear species from Vancouver Island, on the Pacific Northwest Coast of North America

AbstractCompetition between taxa related to climate changes has been proposed as a possible factor in Pleistocene megafaunal extinctions, and here we present isotope evidence of the diets of three co‐existing bear species [black bear (Ursus americanus), brown bear (Ursus arctos), and the now extinct short‐faced bear (Arctodus simus)] from a locale in western North America dating to the Late (Terminal) Pleistocene (~14.5–11.7 ka). The three bear species were found at several sites on Vancouver Island, on the western coast of Canada. To examine the chronological overlap and niche partitioning between these species of bear, we used direct radiocarbon dating, stable isotope analysis and ZooMS proteomic identification methods. Here we present new radiocarbon evidence from Terminal Pleistocene U. americanus, U. arctos and A. simus from several sites on the island, along with both bulk collagen and compound‐specific isotope data for these species. Radiocarbon dates confirm the chronological overlap of Arctodus and both Ursus species in the montane regions of the island at the end of the Pleistocene. Stable isotope data reveal niche differentiation between these species, with U. americanus occupying a distinctly lower trophic position than the other two taxa.

Experimental evaluation of data integration methods for isotopic analysis of uranium with ultra-trace levels using TIMS

Isotopic analysis of ultra-trace levels of uranium (1 ng, 100 pg, 30 pg, and 5 pg) was performed using thermal ionization mass spectrometry (TIMS). The data integration procedure was optimized through experimental evaluation of three data integration methods. In Method I, the isotope ratios of uranium were calculated using pre-integrated ion signal intensities. Statistical integration of the pre-calculated uranium isotope ratios for each data set was performed with and without applying weighting for Methods III and II, respectively. Methods I and III efficiently minimized the deviation of the uranium isotope ratios caused by mass fractionation. The integration range was required to be reduced to 25–100% of the maximum intensity for data sets containing samples with small weights (i.e., 5 pg) for the best accuracy. Method III, with an integration range over 25%, was recommended for individual microparticle analysis by TIMS due to its accuracy, precision, and possibility of uncertainty estimation. The excellent agreement of the isotope ratios of uranium in microparticles (approximately 2–3 μm in diameter) with the certified values verified the applicability of the optimized procedure to the TIMS isotopic analysis of uranium for nuclear safeguards purposes.

Fast and highly sensitive Cd isotopic analyses in low-Cd complex samples with MC-ICPMS based on plasma electrochemical vapor generation

Cd isotopes have provided a powerful tool for better understanding Cd geochemical cycling in soil, water and biological systems. Conventional solution-based MC-ICPMS techniques used for Cd isotopic analysis typically requires time-consuming purification, which greatly limits the wide application of Cd isotope. In this work, a fast, highly sensitive and cost-effective Cd isotopic analysis method has been developed based on plasma electrochemical vapor generation (PEVG) coupled with MC-ICPMS. PEVG enhances sensitivity by more than 6 times compared with conventional pneumatic nebulization (PN) system, allowing Cd analysis to be carried out with samples as low as ∼ 13 ng. Usefully, the tolerance level for organic resin materials and matrix elements (Sn/In/Pd/Zr/Mo/Zn:Cd > 250:1) is greatly improved because of the excellent matrix separation capability inherent to PEVG. This allows simplification of the complex and time-consuming ion-exchange chromatography purification process, achieving a reduction of time by > 20 times compared to conventional two-step Cd purification process. The precision and accuracy of this method were first assessed by measuring NIST 3108 and BGEG-Cd standard under optimum conditions (δ114/110Cd of 0.00 ± 0.06‰ and −1.00 ± 0.06‰ (2sd, n = 25)). The method was also successfully applied to sensitive and fast determination of δ114/110Cd in various reference materials (soil, sediment, and basalt) and environmental samples (pyrite, galena, sphalerite, soils and tap water), validating the applicability of the proposed technique. Owing to the sensitivity, selectivity, low power, and low gas consumption of the PEVG, the proposed PEVG-MC-ICPMS technique provides a much faster and cost-effective approach for the accurate measurement of Cd isotopic compositions in low-Cd complex samples.

Groundwater salinization in a subtropical region, Beihai, southern China: Insights from hydrochemistry and multiple isotopes (H, O, S, Sr)

Groundwater salinization in coastal aquifers is frequently influenced by seawater intrusion, water-rock interaction, and human activities. We selected the Daguansha high productivity mariculture region and used hydrogeochemical, isotopic analysis methods, coupled with water level and quality monitoring, to identify the main groundwater recharging sources, salinization processes, and evolutionary mechanisms of groundwater in Beihai, China. Our conclusions are based on conventional groundwater chemical components and isotope data for hydrogen, oxygen, sulfur, and strontium. Groundwater levels display notable seasonal variations, and the intensity of anthropogenic exploitation is a major factor influencing fluctuations in groundwater level. The variations of total dissolved solids in groundwater correspond to patterns of spatiotemporal variation in deuterium, sulfur, and strontium isotopes. These results indicate groundwater salinization is influenced by a combination of seawater intrusion and infiltration of water from high-productivity mariculture ponds in the Daguansha area. Notably, interlayer leakage between various aquifers in this area was observed. Local anomalies in groundwater characteristics indicate that groundwater salinization is mainly influenced by water from high-productivity mariculture activities. Investigations of the sources and processes underlying groundwater salinization in the Beihai area can provide a scientific basis for groundwater resource management.

An Improved Cr-EA-IRMS Method for the Effective Determination of the Hydrogen Isotopes in Coal Samples.

Hydrogen isotope analysis of coal is an important tool in the geochemical analysis of coal. The traditional method of hydrogen isotope analysis of coal requires the oxidation of organic matter bound hydrogen in coal to water by an oxidizing agent and then its reduction to hydrogen by a reducing agent. This method is time-consuming and laborious, and makes it difficult to cope with the rapid detection of large numbers of samples. The recent development of continuous flow IRMS systems (CF-IRMS) has solved the problem of inefficient analysis, but does not guarantee the quantitative conversion of organic bound H to H2, resulting in inaccurate measured hydrogen isotope values. In this study, for the hydrogen isotope analysis of coal, an alternative continuous flow system (Cr-EA-IRMS) was used to achieve high precision hydrogen isotope measurements of coal samples by filling a quartz reaction tube with Cr. The results obtained by this method (−121.3 ± 1.1‰) for the reference material (GBW11104) are consistent with those obtained by the conventional method (−121.4 ± 0.6‰). Using this method, hydrogen isotope measurements for a variety of imported coals revealed significant differences in the hydrogen isotopes of coals from different coal producing regions including Russia, South East Asia, and Australia. Therefore, the use of hydrogen isotope testing analysis of coal could be a potential means of tracing the origin of coal.

Groundwater dynamic influenced by intense anthropogenic activities in a dried-up river oasis of Central Asia

AbstractIntense anthropogenic activities in arid areas have great impacts on groundwater process by causing river dried-up and phreatic decline. Groundwater recharge and discharge have become hot spot in the dried-up river oases of arid regions, but are not well known, challenging water and ecological security. This study applied a stable isotope and end-member mixing analysis method to quantify shallow groundwater sources and interpret groundwater processes using data from 186 water samples in the Wei-Ku Oasis of central Asia. Results showed that shallow groundwater (well depth &amp;lt; 20 m) was mainly supplied by surface water and lateral groundwater flow from upstream, accounting for 88 and 12%, respectively, implying surface water was the dominant source. Stable isotopes and TDS showed obviously spatiotemporal dynamic. Shallow groundwater TDS increased from northwest to southeast, while the spatial variation trend of groundwater δ18O was not obvious. Surface water and groundwater in non-flood season had higher values of stable isotopes and TDS than those in flood season. Anthropogenic activities greatly affect groundwater dynamics, where land-cover change and groundwater overexploitation are the main driving factors. The findings would be useful for further understanding groundwater sources and cycling, and help restore groundwater level and desert ecosystem in the arid region.

The Stem Sap Flow and Water Sources for Tamarix ramosissima in an Artificial Shelterbelt With a Deep Groundwater Table in Northwest China.

The shelterbelt forest between oases and the desert plays a vital role in preventing aeolian disasters and desertification in arid regions of northwest China. Tamarix ramosissima (T. ramosissima), a typical perennial and native xerophyte shrub in Northwest China, grows naturally and is widely used in building artificial shelterbelt forests. The balance between water consumption and the availability of water determines the survival and growth of T. ramosissima. How T. ramosissima copes with extremely low rainfall and a deep groundwater table remains unknown. To answer this, the transpiration and the water sources of T. ramosissima were investigated by the heat balance and oxygen isotopic analysis method, respectively. Our results show that the daily T. ramosissima stem sap flow (SSF) was positively correlated with air temperature (Ta), photosynthetically active radiation (PAR), and the vapor pressure deficit (VPD). We found no significant relationship between the daily SSF and soil moisture in shallow (0–40 cm) and middle (40–160 cm) soil layers. Oxygen isotope results showed that T. ramosissima mainly sources (>90%) water from deep soil moisture (160–400 cm) and groundwater (910 cm). Diurnally, T. ramosissima SSF showed a hysteresis response to variations in PAR, Ta, and VPD, which suggests that transpiration suffers increasingly from water stress with increasing PAR, Ta, and VPD. Our results indicate that PAR, Ta, and VPD are the dominant factors that control T. ramosissima SSF, not precipitation and shallow soil moisture. Deep soil water and groundwater are the primary sources for T. ramosissima in this extremely water-limited environment. These results provide information that is essential for proper water resource management during vegetation restoration and ecological reafforestation in water-limited regions.

Influence of equilibration time, soil texture, and saturation on the accuracy of porewater water isotope assays using the direct H2O(liquid)–H2O(vapor) equilibration method

The hydrogen and oxygen stable isotopes of water (δ2H and δ18O) are powerful tracers for studying subsurface water flow processes, but the extraction of porewater from unsaturated soil is complex and laborious. The direct liquid–vapor equilibration method (DLVE) for isotope analysis overcomes this challenge by analyzing headspace vapor in isotopic equilibrium with the porewater under closed system conditions. However, the effect of the equilibration time, soil texture, and porewater saturation on isotopic results is not fully understood yet. We tested three differently textured, disaggregated soils (sandy, silty loam and clay) to assess how the equilibration time is impacted by (i) porewater saturation (100%, 80%, 60%, and 40%), and (ii) soil surface area. For all tests, the water loss through diffusion was negligible (<0.3%). The experiments showed that for disaggregated sandy soil, 24 h was a sufficient isotopic equilibration time regardless of water saturation level. Similarly, 24 h was sufficient for kaolinite samples with 100% saturation exhibiting little isotopic variance even after 168 h of equilibration. For saturated silty loam with 2% organic carbon content, 96 h was the optimal equilibration time, whereas saturated silty loam with 4% organic carbon content did not reach isotopic equilibrium by 168 h. The optimal equilibration time increased depending on whether soil samples were disaggregated or kept in a core cutter. Inconclusive results for silty soils with organic carbon revealed the need to further investigate the possible influence of organic carbon on the DLVE method.

Online determination of mercury isotopic compositions at ultratrace levels by automated purge and trap coupled with multicollector inductively coupled plasma-mass spectrometry

This study reports a sensitive online method for Hg isotope analysis at ultratrace levels by automated P&amp;T-MC-ICPMS.

An efficient method for high-precision potassium isotope analysis in carbonate materials

The developed dual-column chromatographic method can purify K in 100–150 mg carbonate materials with satisfactory recovery (∼100%) and negligible blank (∼30 ng) for high-precision K isotope analysis using MC-ICP-MS.

Isotopic Analysis by Laser Ablation Solution Sampling MC-ICP-MS─An Example of Boron.

Using boron as a test analyte, laser ablation (LA) solution sampling multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is proposed and validated as a fast method for isotopic analysis in natural liquids and digested samples without any prior purification process. We demonstrated that the solution reference standard can be used as a bracketing standard for in situ δ11B analysis in solids. Based on a sensitivity enhancement of 8- to 9-fold, all testing solutions were diluted in a 5% (v/v) NH3·H2O instead of classical 2% (v/v) HNO3. With a discrete and minimal sample solvent loading by the LA sampling strategy, it produces nearly "dry" plasma conditions that tolerate the sample matrix remarkably. The memory effect, one of the most difficult challenges in boron analysis, was dramatically eliminated with only 15 s wash time; thus, each analysis took less than 100 s. No significant matrix effects were observed for varying 50-100% boron concentrations in the samples and varying 20-60% NH3·H2O matrix used for the dilution, as well as for samples doped with a 1/100 synthetic seawater matrix. The external precision of δ11B measurements in NIST 951a was ± 0.30‰ (2SD). Good agreement with the values described in literature studies was achieved for δ11B measurements in eight geological reference materials, with precisions between 0.4 and 0.7‰ (2SD), confirming the accuracy of the proposed method. The proposed method offers advantages of simple sample preparation, fast analysis, and little use of chemical reagents.

Recent Progresses in Stable Isotope Analysis of Cellulose Extracted from Tree Rings.

In this work, the challenges and progression in stable isotope investigation, from the analytical tools and technical sample preparation procedures to the dendroclimatological experiments, were reviewed in terms of their use to assess tree physiological responses to environmental changes. Since the isotope signature of whole wood is not always a reliable tool in studying the climate changes, cellulose is often preferred as the study material in paleoclimatic studies. Nevertheless, the isotope analysis of cellulose is challenging due to the difficulty to remove the other wood components (extractives, lignin, pectin, and hemicelluloses). Additionally, in the case of hydrogen isotope analysis, about 30% of the hydrogen atoms of cellulose are exchanged with the surrounding water, which complicates the isotope analysis. In recent years, more automated isotope analysis methods were developed based on high temperature pyrolysis of cellulose, followed by the chromatographic separation of H2 from CO and by their individual isotope analysis using isotope ratio mass spectrometry. When used to investigate climate factors, the combined isotope analysis δ13C and δ18O appears to be the most promising isotope tool. In contrast, the role of δ2H values is yet to be elucidated, together with the development of new methods for hydrogen isotope analysis.

Determination of stable nitrogen isotopic ratios of nitrate ions in ammonium nitrate.

Ammonium nitrate (AN) is one of the most commonly used explosives in criminal cases. The comparison and source-tracing of AN is important for investigation of attribution and fingerprinting of an explosive used at different events. The stable isotope signature of AN is an important index for comparison and tracing. However, the characteristics of the stable nitrogen isotopic ratios of AN (δ15 NNH4NO3 ) alone are not sufficient to achieve a fine comparison between different AN samples. To increase the comparison index and further improve the discriminability between stable nitrogen isotopic ratios of different ANs, a method of isolation and analysis of nitrate ions in AN was established using stable-isotope-ratio mass spectrometry (IRMS). The method was based on the principle that strong alkali react with AN to produce ammonia and nitrate. After the isolation, stable nitrogen isotopes of nitrate ions (δ15 NNO3 ) were obtained using IRMS, and then the stable nitrogen isotopes of ammonium ions from AN (δ15 NNH4 ) was calculated according to the principle of mass balance. The results show that the method is effective for the isolation of nitrate ions without notable isotope fractionation. The developed method was applied to analyze and discriminate AN samples from eight different cities in China. Three samples out of the initial eight AN samples with similar δ15 NNH4NO3 values were further distinguished by their δ15 NNH4 and δ15 NNO3 values. The isolation and stable-nitrogen isotopic analysis method developed for nitrate ions in AN is simple and effective, thereby increasing the discriminability of the stable isotope ratios in AN.

Evaluation of electrothermal vaporization for sample introduction aiming at Cu isotopic analysis via multicollector-inductively coupled plasma mass spectrometry

A new method for Cu isotopic analysis was developed using a commercially available electrothermal vaporization (ETV) device coupled to multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS).The method demonstrated potential for the isotopic analysis of microsamples (e.g., 5 μL) in a biological context. For example, Cu isotopic analysis of NIST 3114 (diluted to 1 mg L−1 Cu) using self-bracketing provided average δ65Cu values of 0.00 ± 0.17‰ (2SD, n = 10) and internal precision values of 712 ppm. In order to achieve this level of accuracy and precision, it is critical to properly deal with the short transient signals generated by the ETV-MC-ICP-MS, which implies using point by point calculations and time lag detector correction (TDC), as well as a criterion to reject potential outliers.The results of this technique were compared with the results obtained via femtosecond-laser ablation-MC-ICP-MS using the same pre-treated serum samples. No significant differences were observed among the results obtained in both cases, while external precision was 0.26‰ for ETV-MC-ICP-MS and 0.24‰ for fs-LA-MC-ICP-MS, expressed as median value of 2SD (n = 27), further proving the usefulness of the approach proposed in this context, as the use of ETV results in a more straightforward approach.

Method for derivatization and isotopic analysis of the insensitive munition compound 3-nitro-1,2,4-triazol-5-one (NTO)

This paper describes an offline low-temperature derivatization method combined with gas chromatography-isotope ratio mass spectrometry (GC-IRMS) to enable compound-specific isotope analysis (CSIA) of C and N in the explosive compound 3-nitro-1,2,4-triazole-5-one (NTO). NTO is being used widely as a component of insensitive munition (IM) composites such as IMX-101, a formulation that is being used to replace the more shock sensitive TNT in artillery shells. The alkylation of NTO with methyl iodide (MeI) as the derivatization reagent was performed in acetone solution at room temperature using triethylamine (Et3N) as a base catalyst. The methylated product of NTO derivatization was identified as 4-methyl-3-nitro-1,2,4-triazol-5-one (MNTO). Accurate and reproducible results were achieved by systematic optimization of MeI and Et3N concentrations and reaction time. Isotopic values of MNTO obtained by GC-IRMS were normalized against those of two 2,4-dinitroanisole (DNAN) in-house reference materials that had been calibrated with isotopic standard reference materials, USGS40 and USGS41a. The resulting method detection limit for derivatization/GC-IRMS of NTO was 788ng of NTO, yielding a precision of ±0.3‰ for both δ13C and δ15N values in good agreement with δ13C and δ15N values for NTO determined by elemental analyzer-IRMS.

A New H–O Isotope Analysis Method for Water in Inclusions of Oxygen‐free Minerals

A New H–O Isotope Analysis Method for Water in Inclusions of Oxygen‐free Minerals