Abstract
A spark-source mass spectrometric (SSMS) method capable of determining traces of hydrogen in micro-volumes of metals was developed by using a pointed metal probe technique. The hydrogen background was decreased to μg g −1 levels by the combination of a method in which the sample in the ion source is baked under vacuum at 323–343 K for more than 25 ks and a liquid nitrogen or liquid helium cryogenic pump method. This method was applied to the analysis of austenitic stainless steels at μg g −1 hydrogen levels, and the relative standard deviation was within 20% for samples with hydrogen concentrations ranging from 2 to 4 μg g −1. The relative sensitivity coefficent was 2.3 (Fe=1).
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