Abstract
Free chlorine evolved during the high-frequency induction furnace combustion of saline sediments at >1500°C interfered very seriously in the iodimetric titration of liberated sulphur dioxide. Remedies based on absorption of chlorine on copper, antimony and other traps were only partly successful; copper was the most efficient but the loss of titratable sulphur was still very large. Sample desalination with refluxing anhydrous methanol in a Soxhlet extractor was the only method found to give satisfactory performance. This procedure was successful for a broad range of salinity values (reference sample mixed with sodium chloride in ratios of 0.09–1.6) without affecting the sulphur minerals present. The procedure showed excellent precision and good agreement with the “best” values available for the USGS MAG-1 Marine Mud (0.40% S) with a relative standard deviation of 1.29%. Iodimetric determination of sulphur in salt core samples (with the sediment in minor proportions) would also be possible.
Published Version
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