TY - JOUR
T1 - Quantitative Analysis of Hydrogen in High-Hydrogen-Content Material of Magnesium Hydride via Laser-Induced Breakdown Spectroscopy
AU - Imashuku, Susumu
AU - Kamimura, Takumi
AU - Kashiwakura, Shunsuke
AU - Wagatsuma, Kazuaki
N1 - Funding Information:
Financial support for the present study was provided by JSPS KAKENHI Grant 19K22038. The authors thank Mr. Tomoyuki Chiba of Tohoku University for helping us perform the determination of hydrogen concentration in MgH samples using the inert gas fusion/gas chromatograph. 2
Publisher Copyright:
Copyright © 2020 American Chemical Society.
PY - 2020/8/18
Y1 - 2020/8/18
N2 - An analytical approach that can rapidly determine a wide range of hydrogen concentration in solid-state materials has been recently demanded to contribute to the hydrogen economy. This study presents a method for estimating hydrogen concentrations ranging from 0.2 to 7.6 mass % via laser-induced breakdown spectroscopy (LIBS) in a few seconds, with an improvement in the upper limit of determination (7.6 mass %) by approximately 1.3 times compared with a previous work (5.7 mass %). This extension of the determinable concentration range was achieved by measuring the emission intensity at 656.28 nm from the sample in a helium atmosphere at 3000 Pa under focused laser irradiation and by reducing the water residues in both the sample and gas line of the LIBS system. The as-determined hydrogen concentrations in magnesium hydride (MgH2) samples agreed well with those estimated through inert gas fusion/gas chromatography. The calibration curve for LIBS analysis was acquired by measuring the emission intensity at 656.28 nm of standard Mg/MgH2 mixtures containing various hydrogen concentrations (0, 0.1, 0.2, 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, and 7.6 mass %). Results indicated that the proposed LIBS-based method is applicable to the rapid quantitative analysis of hydrogen in hydrogen-containing material of MgH2.
AB - An analytical approach that can rapidly determine a wide range of hydrogen concentration in solid-state materials has been recently demanded to contribute to the hydrogen economy. This study presents a method for estimating hydrogen concentrations ranging from 0.2 to 7.6 mass % via laser-induced breakdown spectroscopy (LIBS) in a few seconds, with an improvement in the upper limit of determination (7.6 mass %) by approximately 1.3 times compared with a previous work (5.7 mass %). This extension of the determinable concentration range was achieved by measuring the emission intensity at 656.28 nm from the sample in a helium atmosphere at 3000 Pa under focused laser irradiation and by reducing the water residues in both the sample and gas line of the LIBS system. The as-determined hydrogen concentrations in magnesium hydride (MgH2) samples agreed well with those estimated through inert gas fusion/gas chromatography. The calibration curve for LIBS analysis was acquired by measuring the emission intensity at 656.28 nm of standard Mg/MgH2 mixtures containing various hydrogen concentrations (0, 0.1, 0.2, 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, and 7.6 mass %). Results indicated that the proposed LIBS-based method is applicable to the rapid quantitative analysis of hydrogen in hydrogen-containing material of MgH2.
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U2 - 10.1021/acs.analchem.0c01479
DO - 10.1021/acs.analchem.0c01479
M3 - Article
AN - SCOPUS:85089499628
SN - 0003-2700
VL - 92
SP - 11171
EP - 11176
JO - Analytical Chemistry
JF - Analytical Chemistry
IS - 16
ER -