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Hydrogen determination in welded specimens by carrier gas hot extraction—a review on the main parameters and their effects on hydrogen measurement

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Abstract

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).

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Notes

  1. by pressing “Ctrl -Y” in the Bruker G4/G8 control software and setting the limits manually by using the arrow keys. This is also written in the apparatus’ manual.

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Acknowledgements

The authors want to thank Mr. Michael Richter for the machining of the manifold specimens. Mrs. Stefanie Groth and Mr. Jörg Steger are thanked for assistance in performing the electrochemical charging experiments. Mr. Enrico Steppan is thanked for the fruitful discussions and keeping the lab running.

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Authors and Affiliations

  1. Bundesanstalt für Materialforschung und -prüfung (BAM), Unter den Eichen 87, 12205, Berlin, Germany

    Michael Rhode, Thomas Schaupp, Tobias Mente, Thomas Boellinghaus & Thomas Kannengiesser

  2. Institute for Materials Science and Joining Technology, Otto-von-Guericke University, Universitätsplatz 2, 39105, Magdeburg, Germany

    Michael Rhode & Thomas Kannengiesser

  3. Institute for Failure Analysis and Failure Prevention (ISSV), Helmut Schmidt University, Holstenhofweg 85, 22043, Hamburg, Germany

    Christoph Muenster

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  1. Michael Rhode
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Correspondence to Michael Rhode.

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Recommended for publication by Commission II - Arc Welding and Filler Metals

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Rhode, M., Schaupp, T., Muenster, C. et al. Hydrogen determination in welded specimens by carrier gas hot extraction—a review on the main parameters and their effects on hydrogen measurement. Weld World 63, 511–526 (2019). https://doi.org/10.1007/s40194-018-0664-9

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