S. Halas et J. Szaran, Low-temperature thermal decomposition of sulfates to SO2 for on-line S-34/S-32 analysis, ANALYT CHEM, 71(15), 1999, pp. 3254-3257
We describe a fast, inexpensive, and safe method of direct SO2 extraction f
rom BaSO4 for sulfur isotopic analysis by mass spectrometry. Only two reage
nts are used: (1) pure NaPO3, which is mixed with BaSO4 sample, and (2) Cu
foil, from which reaction boats are manufactured. The extraction precedes i
n the Cu boat placed into a quartz tube connected to a vacuum line. The boa
t is heated to 650-700 degrees C while pure SO2 produced is collected in a
"cold finger". Reaction is complete in 7-10 min. We have proven by means of
O-18-enriched BaSO4 specimens that the oxygen isotopic composition of the
SO2 is totally controlled by O-18 content in NaPO3, when the weight ratio o
f the reagent to sample exceeds 6:1. The method described can be used for "
on-line" SO2 preparation for isotopic analysis.