Seven different dissolution
methods proposed in the literature
to prepare oil samples for metal analysis by inductively coupled plasma
optical emission spectrometry (ICP-OES) were evaluated for V, Ni,
Fe, and Ca analysis of bitumen. The dissolution methods evaluated
were direct dilution, dry ashing, sulfated ashing, ultrasound assisted
extraction, extraction induced emulsion breaking, detergentless microemulsification,
and acid decomposition in closed vessels. The types of bitumen samples
evaluated were raw bitumen, bitumen with emulsified water, and diluted
bitumen. Only direct dilution and sulfated ashing could be recommended
for the dissolution of all types of bitumen samples to quantify V
and Ni content. Of these two methods, only sulfated ashing resulted
in samples with good storage stability. Typical values for these elements
in raw Athabasca bitumen were 224–226 (±14) μg V/g
and 94 (±4) μg Ni/g. No firm recommendation about the most
appropriate dissolution methods for analysis of Fe and Ca in bitumen
could be made, and the values were typically around 10 μg/g
or less for both Fe and Ca. When bitumen was stored as diluted bitumen
in a toluene solution, it was found that 40–50% of the V-containing
species separated from the bulk solution during a 28 day storage period.
Over the same storage period <20% of the Ni-containing species
separated from the bulk solution. These observations are relevant
to bitumen upgrading, and some implications for metal removal from
bitumen were discussed.