The ketone and aldehyde diperoxide (Figure 1 and Figure 2) of the type illustrated in Scheme 2 was prepared from the acid catalysed oxidation of different types of ketones or aldehydes with hydrogen peroxides (about 60% concentration) at temperatures below -10°C (Scheme 1) (Cafferatta et al., 1984, 1986, 1990, 1991, 1995; Jorge et al., 2000, 2001, 2002; Leiva et al., 2001).