Preparation of SF[sub 6] for sulfur isotope analysis by laser heating sulfide minerals in the presence of F[sub 2] gas

Journal Article · Wed Sep 01 04:00:00 EDT 1993 · Geochimica et Cosmochimica Acta; (United States)

DOI:https://doi.org/10.1016/0016-7037(93)90499-M· OSTI ID:5437308

Rumble, D; Hoering, T C; Palin, J M ^[1]

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1. Geophysical Lab., Washington, DC (United States)

The feasibility of in-situ fluorination of sulfide minerals for sulfur isotope analyses has been demonstrated. Laser fluorination of powdered samples, previously analyzed by conventional bulk SO[sub 2] or BrF[sub 5] methods, verifies that comparable precision and accuracy can be achieved with the new method. The [delta][sup 34]S[sub CDT] and [delta][sup 33]S[sub CDT] values of powdered samples are independent of F[sub 2] gas pressure over a range of from 15 to 120 torr. Furthermore, [delta][sup 34]S[sub CDT] values are independent of SF[sub 6] yields from 40 to 100% for powders that do not fluorinate spontaneously at room temperature. The precision of replicate analyses of powdered pyrite, troilite, chalcopyrite, sphalerite, galena, acanthite, and greenockite is typically 0.1-0.2[per thousand]. Interlaboratory comparisons of previously analyzed powders agree as closely as 0.1[per thousand] and disagree by as much as 0.8[per thousand] over a range of [delta][sup 34]S[sub CDT] from [minus]30 to +34[per thousand]. The technique of in-situ laser fluorination was validated by comparison of analyses of side-by-side laser craters and powders from drill holes in polished sulfide mineral surfaces. For isotopically homogeneous samples, laser craters and drill hole powders agree within 0.1-0.3[per thousand] for both [delta][sup 34]S[sub CDT] and [delta][sup 33]S[sub CDT], depending on the mineral analyzed.

• OSTI ID: 5437308
• Journal Information: Geochimica et Cosmochimica Acta; (United States), Journal Name: Geochimica et Cosmochimica Acta; (United States) Vol. 57:18; ISSN GCACAK; ISSN 0016-7037
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102* -- Chemical & Spectral Procedures
CHEMICAL ANALYSIS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
ELEMENTS
EVEN-EVEN NUCLEI
EVEN-ODD NUCLEI
FLUORIDES
FLUORINE
FLUORINE COMPOUNDS
HALIDES
HALOGEN COMPOUNDS
HALOGENS
HEATING
ISOTOPES
LASER-RADIATION HEATING
LIGHT NUCLEI
MINERALS
NONMETALS
NUCLEI
PLASMA HEATING
QUANTITATIVE CHEMICAL ANALYSIS
STABLE ISOTOPES
SULFIDE MINERALS
SULFUR 33
SULFUR 34
SULFUR COMPOUNDS
SULFUR FLUORIDES
SULFUR ISOTOPES
SYNTHESIS