The extremely high selectivity of the newly developed ozone-sulfur che
miluminescence detector (SCD) coupled with controlled-temperature pyro
lysis, was applied to the qualitative and semiquantitative determinati
on of sulfur forms in coal. Pyrolysis products from the heating of a s
ulfur-containing solid sample were swept directly through a high-tempe
rature conversion tube and into the SCD to yield a strong signal. Upon
heating the pyrolysis tube from room temperature to 700 degrees C, se
veral distinct peaks were observed by the SCD, identified as being due
to aliphatic sulfides and thiols, elemental sulfur, simple thiophenes
, pyrite and complex thiophenes. Standard additions of pure inorganic
substances provided semiquantitative determination. Three coals were e
xamined and could be quickly and easily distinguished by their sulfur
forms. The results are compared with those of other pyrolysis methods.