Calibration capacity of hot-pressed hydrogen standards for glow discharge optical emission and mass spectrometry

Highlights: • Hot-pressed Cu and TiH₂ powder mixtures are useful for calibration of hydrogen in GD-OES and GD-MS • TiH₂ is stable in Cu matrix for 20 min at 600 °C and 478 MPa • The dependency of sputtering rate of two-phase materials on mixture was revealed Mixed copper and titanium hydride powder was hot-pressed and characterized by Carrier Gas Hot Extraction, X-Ray Diffraction, Thermal Gravimetric Analysis coupled with Mass Spectrometry, and Scanning Electron Microscopy. The hot-pressed and five conventional samples were applied for calibration of hydrogen in Glow Discharge Optical Emission and Mass Spectrometry. Up to the introduction of 15 ng/s hydrogen the emission yield model is useful in Glow Discharge Optical Emission Spectrometry. A correlation between saturation and even reversal of the emission yield of the spectral lines H121, H486 and H656 and low sputtering rates was found. Hydrogen effects exist for the spectral lines of Cu(II) 219 and Ti(I) 399. In Glow Discharge Mass Spectrometry, a linear dependency of the ¹H ion current on the sputtered mass per time exists over the total range of hydrogen content investigated. Hydrogen effects also exist for the sensitivity of ⁴⁸Ti and ⁶³Cu. The sputtering rate of two-phase materials depends linearly on the sputtered mass per time of one phase, which allows the sputtering rate of two-phase materials with known composition to be predicted.