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The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50 µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2‐x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2‐x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA‐TCD and VHE‐MS.