Analysis of Sulfur Isotope Composition of Gypsum Samples by Elemental Analyzer-Isotope Mass Spectrometry

GAO Jian-fei; XU Yan-ming; FAN Chang-fu; HU Bin; LI Yan-he

doi:10.15898/j.cnki.11-2131/td.201908120128

Rock and Mineral Analysis > 2020 > 39(1): 53-58. > DOI: 10.15898/j.cnki.11-2131/td.201908120128

GAO Jian-fei, XU Yan-ming, FAN Chang-fu, HU Bin, LI Yan-he. Analysis of Sulfur Isotope Composition of Gypsum Samples by Elemental Analyzer-Isotope Mass Spectrometry[J]. Rock and Mineral Analysis, 2020, 39(1): 53-58. DOI: 10.15898/j.cnki.11-2131/td.201908120128

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Analysis of Sulfur Isotope Composition of Gypsum Samples by Elemental Analyzer-Isotope Mass Spectrometry

1.
Key Laboratory of Metallogeny and Mineral Assessment, Ministry of Natural Resources; Institute of Mineral Resources, Chinese Academy of Geological Sciences, Beijing 100037, China
2.
Qingdao Geological Engineering Survey Institute(Qingdao Geological Exploration and Development Bureau), Qingdao 266071, China

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Received Date: August 11, 2019
Revised Date: September 20, 2019
Accepted Date: October 20, 2019
Published Date: December 31, 2019

Abstract

HIGHLIGHTS
(1) Gypsum powder mixed with V₂O₅ was wrapped in a tin cup, and the sulfur isotope compositions were directly determined by continuous flow EA-IRMS method.

(2) The feasibility of direct online analysis of calcium sulfate samples using EA-IRMS was verified through sulfur isotope results of 13 gypsum samples.

(3) Compared with the conventional method, the direct online analysis had the advantages of fast analysis, small sample amount and simple operation.

ABSTRACT

BACKGROUNDThe conventional method for the measurement of sulfur isotopes in sulfate includes mainly barite conversion coupled with dual-inlet SO₂ methods. These methods are facile and reliable. However, the large amounts of samples, the length of time needed, the laborious experimental work, and complicated preprocessing are impractical for the development direction of micro-analysis.
OBJECTIVESTo develop a method for determination of sulfur isotope compositions in gypsum directly through continuous flow elemental analyzer-isotope mass spectrometry (EA-IRMS).
METHODSTwo different preparation methods were used. (1) Direct measurement of sulfur isotopes was carried out by mixing calcium sulfate powder with V₂O₅ in a tin cup using EA-IRMS. (2) Calcium sulfate was fully dissolved in deionized water. The precipitation reagent BaCl₂ was added to the liquid in which the calcium sulfate sample was dissolved. After the precipitated barium sulfate was filtered out, it was washed 2 to 3 times with deionized water. Samples were dried and mixed with V₂O₅ in a sealed tin cup and then determined by mass spectrometry.
RESULTSThe δ³⁴S values of 13 gypsum samples ranged from -20‰ to -30‰, and the results from replicate measurements were compared for these two methods, yielding the absolute difference in δ values were 0.0-0.2 permil, indicating that the sulfur isotope ratios of the same sample were basically identical.
CONCLUSIONSCompared with the conventional analysis method, the application of 'no pretreatment' to analyze the sulfur isotopes of gypsum was conducted successfully. Adding V₂O₅ to samples directly, during the process of instantaneous combustion, the oxygen in calcium sulfate are substituted by the external oxygen in V₂O₅ and oxygen gas, and the obtained oxygen of SO₂ gas is uniform. Therefore, sulfur isotope ratios of SO₂ can completely represent those of the calcium sulfate, making it unnecessary for oxygen isotope correction. The direct online analysis of sulfur isotopes in calcium sulfate samples using EA-IRMS is verified to be feasible.
- calcium sulfate,
- sulfur isotope,
- elemental analyzer-isotope mass spectrometry,
- sample pretreatment

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Analysis of Sulfur Isotope Composition of Gypsum Samples by Elemental Analyzer-Isotope Mass Spectrometry

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