Simultaneous Determination of Total Carbon, Nitrogen, Hydrogen and Sulfur in Twenty‐seven Geological Reference Materials by Elemental Analyser

A method for the determination of total sulfur in geological materials by inductively coupled plasma‐optical emission spectrometry (ICP‐OES) is described. We show that good results were obtained using this method even for sample types with very low (< 20 μg g−1) sulfur concentration (e.g., peridotite). Sulfur was determined in fifteen geological reference materials with different sulfur contents. For reference materials with certified sulfur contents, the ICP‐OES method gave results in excellent agreement with certified values, and uncertainties better than 4% RSD. ICP‐OES results for sulfur in other reference materials yielded RSDs better than 10%, where S concentrations were > 100 μg g−1 (except for diabase W‐2a, 16% RSD). Reference materials with lower sulfur contents (< 40 μg g−1) showed much higher RSDs (17–18%). Except for RMs with certified values for sulfur, most data obtained by the combustion infrared detection method generally showed higher concentrations than those measured by ICP‐OES and a better RSD (≤ 8% for all materials except DTS‐2b).

Section: Resultssupporting

confidence: 90%

Determination of Total Sulfur in Fifteen Geological Materials Using Inductively Coupled Plasma‐Optical Emission Spectrometry (ICP‐OES) and Combustion/Infrared Spectrometry

Ackerman

Rohovec

Šebek

2012

“…(), Go ‐ Govindaraju (), Gl ‐ Glasby et al . (), H&G ‐ Hu and Gao (), H&P ‐ Hall and Pelchat (), K ‐ Kubota (), Ma ‐ Marin et al . (), M&N1 ‐ Makishima and Nakamura (), M&N9 ‐ Makishima and Nakamura (), M&V ‐ Michel and Villemant (), Ok ‐ Okai et al .…”

Section: Resultsmentioning

confidence: 99%

Abundances of Sulfur, Selenium, Tellurium, Rhenium and Platinum‐Group Elements in Eighteen Reference Materials by Isotope Dilution Sector‐Field ICP‐MS and Negative TIMS

Wang

Becker

2014

Geological reference materials (RMs) with variable compositions and NIST SRM 612 were analysed by isotope dilution mass spectrometry for bulk rock concentrations of chalcogen elements (sulfur, selenium and tellurium), rhenium and platinum‐group elements (PGEs: Ru, Pd, Os, Ir and Pt), including the isotope amount ratios of 187Os/188Os. All concentrations were obtained from the same aliquot after HCl‐HNO3 digestion in a high pressure asher at 320 °C. Concentrations were determined after chemical separation by negative TIMS, ICP‐MS and hydride generation ICP‐MS (Se, Te). As in previous studies, concentrations of the PGEs in most RMs were found to be highly variable, which may be ascribed to sample heterogeneity at the < 1 g level. In contrast, S, Se and Te displayed good precision (RSD < 5%) in most RMs, suggesting that part of the PGE budget is controlled by different phases, compared with the chalcogen budget. The method may minimise losses of volatile chalcogens during the closed‐system digestion and indicates the different extent of heterogeneity of chalcogens, Re and PGEs in the same sample aliquot. OKUM, SCo‐1, MRG‐1, DR‐N and MAG‐1 are useful RMs for the chalcogens. NIST SRM 612 displays homogenous distribution of S, Se, Te, Pt and Pd in 30 mg aliquots, in contrast with micro‐scale heterogeneity of Se, Pd and Pt.

“…, Okai et al . , Kubota ). Table lists recommended values for the geochemical reference materials analysed in this study.…”

Section: Resultsmentioning

confidence: 99%

Sulfur Concentration in Geochemical Reference Materials by Solution Inductively Coupled Plasma‐Mass Spectrometry

Erdman

Lee

Yang

et al. 2013

With implications for the origin of ore deposits, redox state of the atmosphere, and effects of volcanic outgassing, understanding the sulfur cycle is vital to our investigation of Earth processes. However, the paucity of sulfur concentration measurements in silicate rocks and the lack of well-calibrated reference materials with concentrations relevant to the rocks of interest have hindered such investigations. To aid in this endeavour, this study details a new method to determine sulfur concentration via high mass resolution solution inductively coupled plasma-mass spectrometry (ICP-MS). The method is based on an aqua regia leach, involving relatively rapid sample preparation and analysis, and uses small test portion masses (< 50 mg). We utilised two independently prepared standard solutions to calibrate the analyses, resulting in 4% accuracy, and applied the method to eight geochemical reference materials. Measurements were reproducible to within~10%. Sulfur concentrations and isotopes of six reference materials were measured additionally by elemental analysercombustion-isotope ratio mass spectrometry to independently evaluate the accuracy of the ICP-MS method. Reference materials that yielded reproducible measurements identical to published values from other laboratories (JGb-1, JGb-2 and MAG-1) are considered useful materials for the measurement of sulfur. Reference materials that varied between studies but were reproducible for a given test portion perhaps suffer from sample heterogeneity and are not recommended as sulfur reference materials.