Hydrogen and Deuterium Analysis Using Laser-Induced Plasma Spectroscopy

使用激光诱导等离子体光谱分析氢和氘

基本信息

批准号：
17550077
负责人：
KAGAWA Kiichiro
金额：
$ 2.05万
依托单位：
University of Fukui
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2005
资助国家：
日本
起止时间：
2005 至 2006
项目状态：
已结题

项目摘要

Laser-induced plasma spectroscopy (LIPS) has been expanded in many fields as a rapid quantitative analytical tool. However, little work has been reported on the analysis of hydrogen as impurity in solid materials because ordinary. LIPS is conducted at 1 atm, under which condition hydrogen emission (Hα) undergoes a severe line broadening and drastic diminishing in emission efficiency. In this study we have demonstrated that H analysis can be realized by controlling some conditions in the laser plasma production, such as ambient gas pressure, gas kind and laser focusing. As one of the application of H analysis, we have made H analysis in Zicaloy sample, which is very important issue in the nuclear power station industry.1) H analysis at reduced pressureIt has been found that helium low pressure around 10 Torr offers a good condition for H analysis in solids. High sensitive and high precision analysis was demonstrated on zicaloy samples (containing H in the range from 200ppm and 4300ppm) by employing rather extreme defocusing condition (-45mm for f=200m lens) for YAG laser irradiation(140mJ), presenting a good linear calibration curve with a detection limit of about 50ppm.2)H analysis in He gas at 1 atmAnother excitation technique was developed; namely, excitation through He metastable-state(He*). For this purpose, YAG laser pulse was intentionally focused at 10mm above the sample surface so as to induce a gas breakdown plasma, where He*atoms are produced, together with the laser ablation from the sample surface. It was confirmed that a good linear calibration curve is available even in this case with a detection limit of around 100ppm.3) Deuterium analysisWe have also proved that H and D(deuterium) analysis can be made simultaneously by suppressing the spectra broadening of Hα and Dα., nevertheless the peak wavelength shift is only 0.18nm..

激光诱导的血浆光谱法（LIPS）已在许多领域扩展，作为快速定量分析工具。但是，由于普通的氢而分析氢作为杂质的分析几乎没有报道。嘴唇在1个大气压下进行，在这种情况下，氢发射（Hα）经历了严重的线扩大和发射效率的急剧下降。在这项研究中，我们已经证明，可以通过控制激光血浆产生的某些条件来实现H分析，例如环境气压，气体种类和激光聚焦。作为H分析的应用之一，我们在Zicaloy样品中进行了H分析，这在核电站行业中非常重要。1）H分析在降压降低时，Helium弱压大约10 TORR为固体中的H分析提供了良好的条件。通过使用相当极端的偏置条件（F = 200m镜头的-45mm）对YAG激光照射（140mJ）使用相当极端的偏置条件（140mJ），在Zicaloy样品中（包含H的H和4300ppm）进行了高敏感和高精度的分析（包含H的H范围），从而呈现了一个良好的线性校准曲线，并具有50pp Mm. 2 Antif at at He Antion at Ancomption He Antion at Antive n at Antive line calibration校准曲线，也就是说，通过他的稳态状态（他*）令人兴奋。为此，有意将YAG激光脉冲聚焦在样品表面上方10mm上，以诱导气体分解等离子体，在该血浆中产生了他*原子，以及从样品表面的激光消融。据证实，即使在这种情况下，也可以使用良好的线性校准曲线，而检测极限约为100ppmm。3）氘分析我们还证明，可以简单地通过抑制Hα和dα的光谱扩展来进行H和D（氘）分析。但是，峰值波长移位绝对只有0.18nm。