This paper compares the performance and limitations of two analytical
methods for samples from the environment: Instrumental Neutron Activat
ion Analysis (INAA) and Inductively Coupled Plasma with Mass Spectrome
try (ICP-MS). A Brazilian river, the Das Velhas, was chosen as the tes
t-site. This river runs through a Fe, Mn and Au mining area. The two m
ethods were initially tested on three international reference material
s: SLRS-3 (riverine water, Research Council Canada), GS-N (granite, AN
RT, France) and SOIL-7 (soil, International Atomic Energy Agency, Vien
na, Austria). Actual river samples (water and sediments) were analysed
next. The INAA and ICP-MS results were generally in good agreement. H
owever, ICP-MS analysis occasionally suffered from random flask contam
ination (e.g. Zn). The concentrations obtained by ICP-MS for certain e
lements (e.g. Zr) were lower than the certified values and results fro
m INAA, probably because the dissolution of their natural forms (oxide
s) was not complete. For INAA, only one irradiation run was used. Some
elements with short half-life radioisotopes (e.g. Mn, Mg or V) and us
ually analysable by NAA were not detected. The results obtained for th
e Das Velhas river showed a strong relationship between mining activit
y and pollutant concentrations. Increased concentrations of certain me
tals corresponded to passage of the river through the industrial minin
g area. The use of both INAA and ICP-MS enabled accurate results for w
ater and sediment samples to be obtained for approximately 50 elements
. For water analysis, ICP-MS was clearly the most convenient method, a
s INAA was handicapped by the effect of radiolysis which prevented irr
adiation of liquid samples. For sediment analysis, sample preparation
time for ICP-MS was time consuming. INAA avoided these problems and co
uld be used as a reference method. Routinely, a particular method was
selected for each element.