干旱区生态环境知识资源中心(Arid): Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments

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DOI	10.1002/rcm.9102
	Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments
	Klipsch, Swea; Herwartz, Daniel; Staubwasser, Michael
通讯作者	Klipsch, S (corresponding author), Univ Cologne, Inst Geol & Mineral, Cologne, Germany.
来源期刊	RAPID COMMUNICATIONS IN MASS SPECTROMETRY
ISSN	0951-4198
EISSN	1097-0231
出版年	2021
卷号	35 期号:14
英文摘要	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 O-2 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 1 sigma SD external reproducibility is 0.12 parts per thousand for Delta O-17(SO4) values on 30 mu mol 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.
类型	Article
语种	英语
开放获取类型	hybrid
收录类别	SCI-E
WOS记录号	WOS:000661178400002
WOS关键词	ATACAMA DESERT ; DELTA-O-18 ; EXCHANGE ; O-2 ; CONSTRAINTS ; NITRATE ; SULFUR ; QUARTZ ; SOILS ; WATER
WOS类目	Biochemical Research Methods ; Chemistry, Analytical ; Spectroscopy
WOS研究方向	Biochemistry & Molecular Biology ; Chemistry ; Spectroscopy
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/351471
作者单位	[Klipsch, Swea; Herwartz, Daniel; Staubwasser, Michael] Univ Cologne, Inst Geol & Mineral, Cologne, Germany
推荐引用方式 GB/T 7714	Klipsch, Swea,Herwartz, Daniel,Staubwasser, Michael. Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments[J],2021,35(14).
APA	Klipsch, Swea,Herwartz, Daniel,&Staubwasser, Michael.(2021).Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments.RAPID COMMUNICATIONS IN MASS SPECTROMETRY,35(14).
MLA	Klipsch, Swea,et al."Optimizing sulfate pyrolysis triple oxygen isotope analysis for samples from desert environments".RAPID COMMUNICATIONS IN MASS SPECTROMETRY 35.14(2021).