Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments
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| Title: | Main Title: Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments |
| Description: | Abstract: Rationale: The triple oxygen isotope composition of sulfate may reveal the formation pathway and depositional sources and may indicate slow biologic cycling in the environment. Pyrolysis mass spectrometry is better suited for large sample workloads during environmental profiling but sufficient precision and a thorough verification of accuracy are required for comparison with higher precision laser fluorination data. Methods: Quantitative sulfate extraction from soil samples at neutral pH, purification, conversation into Ag-sulfate, and pyrolysis mass spectrometry were modified for high sample throughput. Samples were analyzed after pyrolysis in quartz cups and gold capsules in a modified EuroVector model 3000 elemental analyzer. Sample O2 was measured in continuous He-flow after purification by cryo-trapping and chromatography on a Thermo Finnigan MAT253 isotope ratio mass spectrometer. A protocol for routine quality control and data normalization ensures long-term accuracy of the pyrolysis method. Results: The 1σ SD external reproducibility is 0.12‰for Δ17OSO4 values on 30 μmol samples. Careful normalization for a daily analytical session accounts for changing pyrolysis conditions over the course of multiple sessions. The precision and accuracy obtained with quartz cups are comparable with those obtained with gold capsules. Pyrolysis and fluorination data for in-house standards from four laboratories and from an Atacama Desert gypsum-soil profile are identical and demonstrate the accuracy of our simplified method. Conclusions: Pyrolysis of sulfate in quartz cups and a modified simple elemental analyzer setup allows for accurate, precise, fast, cost-efficient, and non-hazardous mass spectrometric analysis. Exchangeability of data from pyrolysis and laser fluorination methods was demonstrated by repeat analysis of standards and natural samples despite high contents of interfering, easily soluble nitrates and chlorides. |
| Identifier: | https://doi.org/10.1002/rcm.9102 (DOI) |
Responsible Party
| Creators: | Swea Klipsch (Author), Daniel Herwartz (Author), Michael Staubwasser (Author) |
| Funding Reference: | Deutsche Forschungsgemeinschaft (DFG): CRC 1211: Earth - Evolution at the Dry Limit |
| Publisher: | John Wiley & Sons Ltd. |
| Publication Year: | 2021 |
Topic
| CRC1211 Topic: | Climate |
| Related Subproject: | C4 |
| Subjects: | Keywords: Stable Isotope Geochemistry, Paleoclimate Proxies |
| Geogr. Information Topic: | Environment |
File Details
| Filename: | Klipsch_et_al_2021_Optimizing_sulfate_pyrolysis_triple_oxygen_isotope_analysis_for_samples_from_desert_environments.pdf |
| Data Type: | Text - Publication |
| File Size: | 1.7 MB |
| Dates: | Submitted: 09.12.2020 Accepted: 08.04.2021 |
| Mime Type: | application/pdf |
| Data Format: | |
| Language: | English |
| Status: | Completed |
Constraints
| Download Permission: | Only Project Members |
| General Access and Use Conditions: | According to the CRC1211DB data policy agreement. |
| Access Limitations: | According to the CRC1211DB data policy agreement. |
| Licence: | [Creative Commons] Attribution 4.0 International (CC BY 4.0) |
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Specific Information - Publication
| Publication Status: | Published |
| Review Status: | Peer reviewed |
| Publication Type: | Article |
| Article Type: | Journal |
| Source: | Rapid Communications in Mass Spectrometry |
| Source Website: | https://analyticalsciencejournals.onlinelibrary.wiley.com/journal/10970231 |
| Issue: | 14 |
| Volume: | 35 |
| Number of Pages: | 11 (1 - 11) |
Metadata Details
| Metadata Creator: | Swea Klipsch |
| Metadata Created: | 14.07.2021 |
| Metadata Last Updated: | 14.07.2021 |
| Subproject: | C4 |
| Funding Phase: | 1 |
| Metadata Language: | English |
| Metadata Version: | V50 |
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| Page Visits: | 118 |
| Metadata Downloads: | 0 |
| Dataset Downloads: | 0 |
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