Quantitative Analysis of Deuterium in Zircaloy Using Double-Pulse Laser-Induced Breakdown Spectrometry (LIBS) and Helium Gas Plasma without a Sample Chamber

• Published in: Analytical chemistry (Washington) Vol. 84; no. 5; pp. 2224 - 2231
• Main Authors: Suyanto, H, Lie, Z. S, Niki, H, Kagawa, K, Fukumoto, K, Rinda, Hedwig, Abdulmadjid, S. N, Marpaung, A. M, Pardede, M, Suliyanti, M. M, Hidayah, A. N, Jobiliong, E, Lie, T. J, Tjia, M. O, Kurniawan, K. H
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 06-03-2012
• Subjects: Analytical chemistry; Calibration; Chemistry; Exact sciences and technology; Hydrogen; Mass spectrometry; Nuclear accidents & safety; Nuclear power plants; Spectrometric and optical methods; Deuterium; In situ; Suppression; Standard; Target; Plant; Emission spectrometry; Sample preparation; Zircaloy; Detection limit; Standard curve; Quantitative analysis; Trace analysis; Vegetals; Melting; Sample; Use; Concentration; Helium; Low energy; Heavy water; Safety measure; Laser pulse; Pulsed laser; Fuel; Alternative method; Laser ablation technique; Laser produced plasma; Application
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/ac202744r

A crucial safety measure to be strictly observed in the operation of heavy-water nuclear power plants is the mandatory regular inspection of the concentration of deuterium penetrated into the zircaloy fuel vessels. The existing standard method requires a tedious, destructive, and costly sample preparation process involving the removal of the remaining fuel in the vessel and melting away part of the zircaloy pipe. An alternative method of orthogonal dual-pulse laser-induced breakdown spectrometry (LIBS) is proposed by employing flowing atmospheric helium gas without the use of a sample chamber. The special setup of ps and ns laser systems, operated for the separate ablation of the sample target and the generation of helium gas plasma, respectively, with properly controlled relative timing, has succeeded in producing the desired sharp D I 656.10 nm emission line with effective suppression of the interfering H I 656.28 nm emission by operating the ps ablation laser at very low output energy of 26 mJ and 1 μs ahead of the helium plasma generation. Under this optimal experimental condition, a linear calibration line is attained with practically zero intercept and a 20 μg/g detection limit for D analysis of zircaloy sample while creating a crater only 10 μm in diameter. Therefore, this method promises its potential application for the practical, in situ, and virtually nondestructive quantitative microarea analysis of D, thereby supporting the more-efficient operation and maintenance of heavy-water nuclear power plants. Furthermore, it will also meet the anticipated needs of future nuclear fusion power plants, as well as other important fields of application in the foreseeable future.