Cl. Gregory et al., AUTOMATED PARTICLE ANALYSIS OF POPULATIONS OF SILVER-HALIDE MICROCRYSTALS BY ELECTRON-PROBE MICROANALYSIS UNDER CRYOGENIC CONDITIONS, Analytical chemistry (Washington), 70(13), 1998, pp. 2551-2559
An automated particle analysis routine is implemented on an electron m
icroprobe for analyzing the chemical composition and projective area o
f populations of individual silver halide microcrystals. An LN2 cryost
age is used to prevent material degradation due to reaction with the i
mpinging electron beam. The background in the EDX spectra is lowered b
y depositing the microcrystals on a carbon-coated copper grid, mounted
in a transmission holder. The IL-alpha/AgL-alpha net X-ray intensity
ratio, obtained from a spectrum-fitting algorithm, is used to determin
e the crystal composition by means of a standard-based calibration cur
ve. The uncertainty on the concentration measurement of individual mic
rocrystals is calculated using the uncertainties on the net X-ray coun
ts and the uncertainties on the calibration curve. The area measuremen
t is optimized by introducing a gray value histogram correction on eac
h individual measurement. Overlapping microcrystals are scrapped from
the analysis by defining a maximum shape factor, against which the sha
pe factor of the microcrystal is tested. To minimize problems with dri
ft of the cryostage, spectrum acquisition is carried out immediately a
fter a single microcrystal has been located, based on the backscattere
d electron image. Several applications are discussed.