Analysis of Hydrogen in Inorganic Materials and Coatings: A Critical Review

Abstract

The currently used bulk analysis and depth profiling methods for hydrogen in inorganic materials and inorganic coatings are reviewed. Bulk analysis of hydrogen is based on fusion of macroscopic samples in an inert gas and the detection of the thereby released gaseous H2 using inert gas fusion (IGF) and thermal desorption spectroscopy (TDS). They offer excellent accuracy and sensitivity. Depth profiling methods involve glow discharge optical emission spectroscopy and mass spectrometry (GDOES and GDMS), laser-induced breakdown spectroscopy (LIBS), secondary ion mass spectrometry (SIMS), nuclear reaction analysis (NRA), and elastic recoil detection analysis (ERDA). The principles of all these methods are explained in terms of the methodology, calibration procedures, analytical performance, and major application areas. The synergies and the complementarity of various methods of hydrogen analysis are described. The existing literature about these methods is critically evaluated, and major papers concerning each method are listed.

Kinetics of Hydrogen Desorption from Yttrium Hydride: The Development of Material Characterization Methods

“…The spatial resolution of the Raman mapping typically ranges from 0.5-6 µm with a 532 nm laser, depending on the objective lens [12]. These spatial resolutions are far better than those of bulk testing methods proposed by Weiss [4]. Therefore, this study showed great progress in probing local hydride content at a microscopic scale, although neutron imaging could still be superior in terms of scan volume and accuracy [5].…”

“…Bulk H content is typically measured by the weight gain of sample before and after hydriding [2], which results in a nominal composition, assuming a uniform microstructure. The other methods for the bulk analysis of H include inert gas fusion, thermal desorption spectroscopy, glow discharge optical emission spectroscopy and mass spectrometry, laser-induced breakdown spectroscopy, secondary ion mass spectrometry, nuclear reaction analysis, and elastic recoil detection analysis [4]. Despite various options for the bulk analysis of H, the local H analysis of bulk specimen at a microscale has been limited.…”

On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis

“…This requires a prescribed relation of volume to surface geometry of the individual material pieces of the PTS, and a prescribed cleaning procedure to be applied immediately prior to weighing, such that the well-defined state is reached for which the certified value applies. Very sophisticated methods, such as photon activation analysis and then removing surface oxygen, can be used to reliably distinguish between oxygen on the surface and in the bulk of the material [20][21][22][23]. For the measurement of "gaseous" components in the candidate material, only direct solid sampling methods can be used, such as glow discharge mass spectrometry (GDMS), carrier gas hot extraction (CGHE), or the combustion method for other non-metallic impurities.…”

Hydrogen and its detection in fusion and fission nuclear materials – a review

“…Despite some of these most common and frequently used techniques having a blind spot for hydrogen, many other techniques are capable of directly measuring and quantifying hydrogen in materials. Excellent reviews have published that contrast a variety of these hydrogen measurement techniques [52][53][54]. Table 3 provides a list of available techniques used for measuring hydrogen in fusion and fission relevant materials.…”

“…The energy spectrum of the emitting alpha particles is measured and used to determine the D inventory in the sample [57]. The reaction yield is proportional to the flux of incident 3 He ions and the cross section [52].…”