Abstract：“0.0 μg/g” was appeared for ultralow hydrogen analysis on the screen of the apparatuses which were based on the principle of impulse-heating fusion. The “zero peak” problem was investigated and discussed systematically. The experiments indicated that, if the graphite duplex crucible was replaced by single crucible, an obvious hydrogen peak could be observed under the same condition. It was the interference peak proved by the test of the 10-point analysis with the self-certification sample. The trial to solve the “zero peak” problem was failed by bath adding tests. But it was successful to solve the problem by other instrument based on induction-heating hot extraction. The induction-heating hot extraction instrument was applied to analyze hundreds of “zero peak” samples. The stable hydrogen peaks could be found in range of 0.1-0.4 μg/g. The instrument was calibrated with both Leco 502-457 and Alpha AR546 certified reference materials with certified value of (0.9±0.4) μg/g and (0.63±0.2) μg/g for hydrogen in steel. It was found that the linearity was good enough. The content of hydrogen in the self-certification steel sample was analyzed by induction-heating hot extraction method, and the results were basically consistent with the certified values of (0.5±0.2) μg/g. The standard deviation (SD,n=10) was 0.07 μg/g. The comparison test for determination of ultralow hydrogen was designed for the rare earth steel samples with the rare earth free steel samples by the impulse-heating fusion and induction-heating hot extraction respectively. “0.0x μg/g” were shown on the screens of the two apparatuses based on impulse-heating fusion for the rare earth steel samples. The fine hydrogen peak with value about 0.4 μg/g were appeared on the screen of the instrument based on induction-heating hot extraction to the same samples. The consistent results of hydrogen analysis were shown to the rare earth free steel samples by the three apparatuses/instruments. Therefore, it was considered that the addition of rare earths could cause negative interference with the analysis of hydrogen in steel. This interference value was very low and could be ignored for induction-heating hot extraction, while it was about 0.2-0.4 μg/g for impulse-heating fusion. In conclusion, the impulse-heating fusion was not suitable for analysis of ultralow hydrogen in steel with mass fraction less than 0.4 μg/g, and should be cautiously applied for the analysis of ultralow hydrogen in steel with mass fraction ranging from 0.4 μg/g to 0.9 μg/g. On the other hand, the induction-heating hot extraction was entirely suitable for ultralow hydrogen analysis in steel which completed the analysis process with the sample keeping solid state. No more negative interference and no “zero peak” phenomenon have been observed from the instrument based on induction heating-extraction.
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