A method for the determination of mercury in solid samples using laser abla
tion coupled with atomic fluorescence spectroscopy has been developed. An N
d-YAG laser was used for ablation and the vaporised and atomised material w
as rapidly led to an atomic fluorescence detector, where excitation and emi
ssion took place. The experimental approach was applied to the assessment o
f different procedures as sensitive as possible for implementing standard a
ddition methods. Calibration curves were recorded using the prepared standa
rds, which exhibited linear ranges between 0.5-100 mu g/g, with excellent r
egression coefficients in all instances (0.9907). The precision, expressed
as RSD %, was 3 and 4% for contents of 1 and 30 mu g/g respectively, in the
same pellet; and 7 and 12% for the same contents and different type of pel
lets. The method has been applied to the determination of mercury in CRM of
sewage sediment and a sludge sample with a known amount of mercury determi
ned by an interlaboratory study. The results obtained show good agreement w
ith those expected.