Determination of Hydrogen in Oxygen Containing Zirconium Hydrides by the Hydrogen Evolution Method
Hydrogen absorbed by pure zirconium can be determined quantitatively with a precision of better than ±1.4 mg or 16 ml per g of the sample, if the latter is dissolved in HP solution, the volume of hydrogen measured, and eq. 5 with R=0 is applied. For hydrogen and oxygen containing solid solutions the residue (ZrO2) left after dissolution has to be collected, weighed, and the full eq. 5 has to be used. The precision of such determinations is about ±16 ml hydrogen per g of the alloy. Oxygen containing samples, if the hydrogen is absorbed at elevated temperatures, always leave the oxygen in the form of ZrO2 which is insoluble in dilute HF solution. However, if hydrogen diffuses into oxygen containing Zr at low temperatures (e.g. room) then it may happen that ZrO2 of smaller grain size (especially in the α-solid solution region) will dissolve completely in the acid and if so, applying eq. 5, will result in too small an amount of absorbed hydrogen. This is a definite limitation of the method. © 1960 Springer Verlag.
M. E. Straumanis et al., "Determination of Hydrogen in Oxygen Containing Zirconium Hydrides by the Hydrogen Evolution Method," Fresenius' Zeitschrift für Analytische Chemie, Springer Verlag, Jan 1960.
The definitive version is available at http://dx.doi.org/10.1007/BF00463946
Materials Science and Engineering
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© 1960 Springer Verlag, All rights reserved.