This work aims to contribute to the study of the Hg-Ba-Cu-O diagram. Genera
lly, we can see that high-temperature superconductor phase diagrams are far
from complete. Of these, the Hg-Ba-Cu-O diagram is very interesting owing
to the high mercury fugacity. However, to study this diagram it is necessar
y to control both the mercury and the oxygen activities. The importance of
this check is evident in the preparation of single-phase samples, where com
petitive phases are often obtained; knowledge of these phases will provide
an improvement. Even the famous superconductor phase HgBa2CuO4+delta is sti
ll the subject of discussion. To study these compounds, thermogravimetric a
nd differential thermal analyses, X-ray diffractometry, scanning electron m
icroscopy and oxygen titration are the most important analyses. In particul
ar, we applied the well known effusion technique, a programmed decompositio
n by the saturated vapour method, rarely used for this purpose.