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Ion-Pair Chromatography Coupled to Inductively Coupled Plasma−Mass Spectrometry (IPC-ICP-MS) as a Method for Thiomolybdate Speciation in Natural Waters

Title data

Lohmayer, Regina ; Reithmaier, Gloria ; Bura-Nakic, Elvira ; Planer-Friedrich, Britta:
Ion-Pair Chromatography Coupled to Inductively Coupled Plasma−Mass Spectrometry (IPC-ICP-MS) as a Method for Thiomolybdate Speciation in Natural Waters.
In: Analytical Chemistry. Vol. 87 (2015) Issue 6 . - pp. 3388-3395.
ISSN 1520-6882
DOI: https://doi.org/10.1021/ac5046406

Abstract in another language

Molybdenum precipitates preferentially under reducing conditions; therefore, its occurrence in sediment records is used as an indicator of paleoredox conditions. Although thiomolybdates (MoO4−xSx2− with x = 1−4) supposedly are necessary intermediates in the process of molybdenum precipitation under anoxic conditions, there is no information about their abundance in natural environments,because of a lack of element-specific methods with sufficientlylow detection limits. Here, we optimized ion-pair chromatographicseparation for coupling to an inductively coupledplasma−mass spectrometry detector (IPC-ICP-MS). 2-Propanol(10%−25% gradient) replaced the previously used acetonitrile (25%−75%) as the solvent, to reduce the carbon load into the plasma. In synthetic solutions, formation of thiomolybdates was found to occur spontaneously in the presence of excess sulfide and the degree of thiolation was highest at pH 7. Excess hydroxyl led to a transformation of thiomolybdates to molybdate. Under acidic to neutral conditions, precipitation of molybdenum and hydrolysis of tetrathiomolybdate were observed. Flash-freezing was found to be suitable to stabilize tetrathiomolybdate, with 2 mM) negatively affected the detection of molybdate, which eluted mainly in the dead volume, but had no negative effect on higher thiolated molybdates. Detection limits were ∼10 nM. With the newly developed IPC-ICP-MSmethod, thiomolybdates were found to form spontaneously in euxinic marine waters after adding a molybdate spike and occur naturally in sulfidic geothermal waters.

Further data

Item Type: Article in a journal
Refereed: Yes
Additional notes: BAYCEER127658
Institutions of the University: Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Earth Sciences > Professorship Environmental Geochemistry Group
Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Earth Sciences > Professorship Environmental Geochemistry Group > Professorship Environmental Geochemistry - Univ.-Prof. Dr. Britta Planer-Friedrich
Faculties
Faculties > Faculty of Biology, Chemistry and Earth Sciences
Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Earth Sciences
Result of work at the UBT: Yes
DDC Subjects: 500 Science
Date Deposited: 03 May 2015 08:56
Last Modified: 03 May 2015 08:56
URI: https://eref.uni-bayreuth.de/id/eprint/12612