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Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in weld joints using a thermal conductivity detector (TCD) for hydrogen measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries (ISO 3690 type B and small cylindrical samples), and factors that additionally influence hydrogen determination. They are namely specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PI-furnace controller, as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up to the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by Evaluation of the recorded data. Generally, independent temperature measurement with dummy specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA).
Hydrogen generally causes lattice distortions and phase transformations when introduced into a metallic crystal lattice. For the investigations reported in this contribution, hydrogen thermal desorption analysis has been carried out to observe the influence of hydrogen desorption on the lattice of super martensitic stainless steel during continuous heating. The lattice expansion parameter and the phase transformations have been monitored during the thermal desorption process, and the influence of hydrogen on such characteristics has been evaluated. It was found that hydrogen has a significant influence on both the lattice parameter and on the thermal expansion. However, hydrogen has no influence on phase transformation during thermal desorption. The hydrogen's desorption behavior in this process was also observed and it turned out that hydrogen desorbs in two stages, i.e., firstly diffusible hydrogen and trapped hydrogen afterward.