Pn. Petrov et al., DETERMINATION OF HYDROGEN IN SILICON, GERMANIUM, ALUMINUM, AND OTHER HIGH-PURITY SUBSTANCES BY HIGH-TEMPERATURE EXTRACTION, Journal of analytical chemistry, 53(2), 1998, pp. 181-190
A comparative analysis of the potential of high-temperature extraction
in a vacuum and in an inert-gas flow was performed. It was shown that
hydrogen can be determined at a level of (1-3) x 10(-6)% using vacuum
extraction, whereas hydrogen at higher concentrations of (5-10) x 10(
-6)% can be determined using high-temperature inert-gas extraction. Th
e fundamentals and procedures of the determination of hydrogen in high
-purity silicon, germanium, aluminum, indium, gallium, tin, lead, cadm
ium, and tellurium were developed. Germanium and silicon were analyzed
by the vacuum heat technique in an open graphite crucible at temperat
ures of 900 and 1100 degrees C, respectively; a cascade graphite cruci
ble at a temperature of 900 degrees C and the vacuum melting technique
were used for analyzing indium, gallium, tin, lead, cadmium, and tell
urium. Aluminum and its alloys were analyzed using the high-temperatur
e inert-gas extraction technique with sample melting (no longer than 1
0-15 s) in the analysis mode natural for the sample. The detection lim
it of hydrogen was found to be (2-6) x 10(-7)% in vacuum extraction an
d (5-7) x 10-7% in high-temperature inert-gas extraction (for a sample
of mass 6-7 g). The blank correction in the vacuum melting method was
0.01-0.03 mu g/min, the limit of determination of hydrogen was found
to be (2-5) x 10(-6)%, and the relative standard deviation of the resu
lts of replicate measurements was 10-15%.