Determination of sulfur in fluid inclusions by laser ablation ICP-MS

Abstract

The quantification capabilities for sulfur microanalysis in quartz-hosted fluid inclusions were investigated with laser ablation (LA) inductively coupled plasma quadrupole mass spectrometry (ICP-Q-MS) and ICP sector field mass spectrometry (ICP-SF-MS) allowing resolution of sulfur from polyatomic interferences. A scapolite mineral sample was used to determine the sulfur concentration in NIST SRM 610 (570 AE 70 mg g À1 ), which was further validated using EPMA and then used as standard reference material for the fluid inclusion analysis. The sulfur concentration in an assemblage of brine inclusions from a quartz-molybdenum vein was determined to be 5900 AE 2000 mg g À1 measuring 17 inclusions with the ICP-SF-MS and 13 inclusions with the ICP-Q-MS instrument. The agreement between the two ICP-MS instruments for sulfur was $5% and well within the overall precision of 35% relative standard deviation. The precision and accuracy was not limited by interferences, but by a so far unknown sulfur contamination source when ablating the host mineral quartz. Due to this contamination, a careful baseline correction is necessary which is described and discussed in detail. Nevertheless, the method developed to determine sulfur maintains the multi-element capabilities for individual fluid inclusions. Limits of detection for sulfur are correlated with the inclusion mass and were found to be $ 30-100 mg g À1 for 60 mm inclusions.

Laser Ablation-Inductively Coupled Plasma Mass Spectrometry for the Characterization of Pigments in Prehistoric Rock Art

“…42,43 Recently, even for the S content, values have been reported. 44 The only elements of the list for which no reference values are available (to the best of the authors' knowledge) are C, Hg, Ir, Ru, and Os. However, no Hg, Ir, Ru, or Os signals above the limit of detection (LOD) were detected for the samples, while C quantification is not expected to provide relevant fingerprinting information (and SEM values for this element were available anyway).…”

“…To correct for the differences in the ablation yields between the samples and the NIST SRM glass standards, the signal from 44 Ca + was used as internal reference, following the formula described in detail by Longerich et al 45 SEM values for the Ca content in every sample were used in these calculations. This calibration strategy (use of NIST glasses and an internal reference of known concentration) has been reported to provide accurate results for any oxygen-rich matrix 46 and, particularly, for carbonates, as is the case here.…”

Interference standard applied to sulfur determination in biodiesel microemulsions by ICP-QMS

“…In addition to such interferences, the high ionization potential of S (10.36 eV), which results in a low ionization efficiency in the plasma (about 14%), contributes to the lower sensitivity of this element in ICP-QMS. 9,14,15 Despite these difficulties, several refinements and improvements have been made on ICP-MS since its introduction in the 1980s. Post-plasma correction methods based on collision and/or reaction processes for interfering ion suppression have been successfully employed.…”

Applications of LA-ICP-MS in the elemental analyses of geological samples

“…The limits of detection vary widely according to the inclusion volume, but range from 1 to 100 ppm for most elements [166]. In recent years, important progress has been made in the analyses of S, Cl and Br in single fluid inclusions by LA-ICP-MS. Guillong et al [13] developed a method to analyze the S content in individual fluid inclusions using scapolite as an external standard and found that the factor that affected the precision and accuracy was not interference, but rather S pollution from an unknown source. Seo et al [167] and Leisen et al [168] reported a method for the analysis of Cl and Br concentrations in single fluid inclusions that involves calibration against NIST glass and/or scapolite.…”