The microdiffusion method published by Brouwer and Murphy([1]) for analysis
of acid volatile sulphide (AVS-chiefly FeS) has been extended to both AVS
and FeS(2)in a two step process. For the first step (AVS analysis), excelle
nt recoveries (similar to 100%) are obtained for Na2S, FeS, PbS, CdS, and Z
nS provided diffusion times are long enough. Recovery from other insoluble
metal sulphides (Ag2S and HgS) were low, while for CuS were variable. In th
e second step, recoveries were similar to 100% for ground, crystalline FeS2
. This work re-emphasises the importance of adding a sufficiently strong re
ducing agent during AVS determination in sediments to prevent oxidation of
S-2-by Fe3+ produced in the acid dissolution of ferric phases. The method i
s amenable to adoption to different apparatus provided recoveries and react
ion times are checked with suitable standards.