An electron microprobe study of the influence of beam current density on the stability of detectable elements in mixed‐salts (isoatomic) microdroplets

SUMMARY This paper shows that a means of accurately measuring beam current during microprobe analysis of inorganic fluid microdroplets is essential, since certain elements were sublimated from such specimens under easily achieved beam current densities, i.e. S at 1·8 nA/μm2, K at 2·5 nA/μm2, Na at 3·5 nA/μm2, P at 5·3 nA/μm2. In comparison, Cl was volatilized even under the mildest conditions used (0·35 nA/μm2), and Ca, Mg and Co were stable under the severest operating conditions (7·1 nA/μm2). Elements were less stable in large (3 μm diameter) droplets than in small (1 μm) droplets under identical irradiation conditions. The onset of volatilization is a direct function of the current delivered per unit area and not of the total integrated dose. The addition of 50 g/l of urea to the mixed-salts (isoatomic) solution, or (a) the mounting of the droplets so that the carbon-celloidin support film was interposed between them and the electron source, and (b) top-coating the droplets with carbon, did not, in general, raise the threshold of volatilization of a given element, but did effectively retard the rate of loss at current densities above the volatilization threshold. A literature survey confirmed that similar losses can occur from biological tissue specimens, albeit at higher beam current densities. Finally, the possibility that local specimen heating during electron/specimen interaction is a cause of element loss during microprobe analysis is discussed.