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:PDF
Language:English
Status:Completed
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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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