L. Ottolini et al., QUANTIFICATION OF LITHIUM, BERYLLIUM, AND BORON IN SILICATES BY SECONDARY-ION MASS-SPECTROMETRY USING CONVENTIONAL ENERGY-FILTERING, Analytical chemistry, 65(15), 1993, pp. 1960-1968
A SIMS procedure for Li, Be, and B quantification in silicates has bee
n developed using the empirical approach of working curves via calibra
tion with standards. Medium- to high-energy secondary ions have been u
sed to reduce matrix effects affecting especially Li/Si ionization and
to improve measurement reproducibility with respect to low-energy ion
analysis for Li, Be, and B. In the case of Be, there has been evidenc
e for a possible reduction of matrix effects, whereas in the case of B
, matrix effects have been evidenced to be rather low at any ion energ
y, and in such a case, the application of a voltage offset has been us
eful only to improve measurement reproducibility. Positive ions of the
isotopes Li-7, Be-9, B-11, and Si-30 (assumed as the matrix reference
isotope), having emission kinetic energies ranging from approximately
75 to 125 eV, have been monitored using an ion microprobe Cameca IMS
4F. The calibration curves hold over extended concentration ranges fro
m ppm to percent level by weight for light elements and silica content
s ranging from a few percent to more than 80% by weight. Precision and
accuracy of the method are generally estimated as better than +/-20%
relative at the ppm level and better than +/-10% relative for element
abundances of tens of ppm for Be and B. As for Li, the whole uncertain
ty in the proposed SIMS procedure is evaluated at about +/-20% (28% fo
r lead crystal glasses). These results have important implications for
more extensive applications of SIMS as a 'routine'' microanalytical a
nd bulk technique for the quantification of Li, Be, and B in silicate
minerals and rocks.