Abstract
Currently, standard samples of hydrogen-metal systems meeting the requirements of glow discharge optical emission spectrometers (GD-OES) are not available on the market. This article describes the preparation of Zr-Nb-H standard samples and the calibration of GD-OES with the usage of these samples. Samples of Zr-2.5Nb were chosen as the material for sample production. The creation procedure includes five main steps: sample preparation (polishing to an average roughness, Ra, of 0.04 m using sandpaper), annealing, hydrogenation, maintenance in an inert gas atmosphere, and characterization of the samples. The absolute hydrogen concentration in the samples was determined volumetrically and calculated from the weight change. The distribution of hydrogen was studied using GD-OES Profiler 2 by Jobin Yvon Emission Horiba Group. As a result of this work, calibration curves of Zr, H, Nb, O, and other elements were obtained. The calibration errors were in the range of 1–5%.
Highlights
Zirconium and its alloys are well-known and established construction materials used in nuclear reactors [1]
It is shown that hydrogen concentrations determined by two different methods have a good correlation
The concentrations of hydrogen calculated from the weight change that have been confirmed by measurement results using a hydrogen analyzer were chosen as the standard concentrations for the calibration of glow discharge optical emission spectrometers (GD-OES)
Summary
Zirconium and its alloys are well-known and established construction materials used in nuclear reactors [1]. Hydrogen can cause phase transformations leading to hydride formation [9,10,11,12,13,14,15,16], interactions with structural defects modifying the plastic activity of materials [17], the interplay with point defects provoking swelling [18,19,20,21], or so-called hydrogen embrittlement. It makes the development of methods for the protection of zirconium alloys from penetration of hydrogen significant. The main part of these studies is an elemental analysis of the materials, which includes qualitative and quantitative analysis
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