Yamamoto, Masahiko; Do, V. K.; Taguchi, Shigeo; Kuno, Takehiko; Takamura, Yuzuru*
Spectrochimica Acta, Part B, 155, p.134 - 140, 2019/05
The emission spectra of technetium (Tc) by liquid electrode plasma optical emission spectrometry have been investigated in this study. From the spectra, 52 emission peaks of Tc were observed in the 250-500 nm wavelength range. All peaks were assigned to the neutral state or singly ionized state. The relative intensities of these peaks were similar to those excited by an electric spark. The strongest intensity peaks were found at 254.3 nm, 261.0 nm, and 264.7 nm. Spectral interferences of coexisting elements in highly active liquid waste of reprocessing stream on those three strongest peaks were investigated using simulated sample. No spectral interferences were observed around the 264.7 nm Tc peak. Therefore, analytical performance using 264.7 nm peak was evaluated. The detection limit, estimated on standard and blank samples in 0.4 M nitric acid, was 1.9 mg/L. The relative standard deviation of Tc standard sample (12.0 mg/L) was 3.8% (N = 5, 1).
Miyabe, Masabumi; Oba, Masaki; Jung, K.; Iimura, Hideki; Akaoka, Katsuaki; Kato, Masaaki; Otobe, Haruyoshi; Khumaeni, A.*; Wakaida, Ikuo
Spectrochimica Acta, Part B, 134, p.42 - 51, 2017/08
Spectroscopic properties of atomic species of plutonium were investigated by combining laser ablation and resonance absorption techniques for the analysis of a plutonium oxide sample. For 17 transitions of Pu atoms and ions, the absorbance, isotope shift, and hyperfine splitting were determined via Voigt profile fitting of the recorded absorption spectra. Three transitions were selected as candidates for analytical use. Using these transitions, we investigated the analytical performance that was attainable and determined a correlation coefficient R2 between the absorbance and plutonium concentration of 0.9999, a limit of detection of 30-130 ppm, and a relative standard deviation of approximately 6% for an abundance of Pu of 2.4%. These results demonstrate that laser ablation absorption spectroscopy is applicable to the remote isotopic analysis of highly radioactive nuclear fuels and waste materials containing multiple actinide elements.
Miyabe, Masabumi; Oba, Masaki; Iimura, Hideki; Akaoka, Katsuaki; Khumaeni, A.*; Kato, Masaaki; Wakaida, Ikuo
Spectrochimica Acta, Part B, 110, p.101 - 117, 2015/08
The dynamic behavior of an ablation plume in ambient gas has been investigated by laser-induced fluorescence imaging spectroscopy. The second harmonic beam from an Nd:YAG laser (0.5-6J/cm) was focused on a sintered oxide pellet or a metal chip of gadolinium. The produced plume was subsequently intersected with a sheet-shaped UV beam from a dye laser so that time-resolved fluorescence images were acquired with an intensified CCD camera at various delay times. The obtained cross-sectional images of the plume indicate that the ablated ground state atoms and ions of gadolinium accumulate in a hemispherical contact layer between the plume and the ambient gas, and a cavity containing a smaller density of ablated species is formed near the center of the plume. At earlier expansion stage, another luminous component also expands in the cavity so that it coalesces into the hemispherical layer. The splitting and coalescence for atomic plume occur later than those for ionic plume. Furthermore, the hemispherical layer of neutral atoms appears later than that of ions; however, the locations of the layers are nearly identical. This coincidence of the appearance locations of the layers strongly suggests that the neutral atoms in the hemispherical layer are produced as a consequence of three-body recombination of ions through collisions with gas atoms. The obtained knowledge regarding plume expansion dynamics and detailed plume structure is useful for optimizing the experimental conditions for ablation-based spectroscopic analysis.
Imazono, Takashi; Suzuki, Yoji; Sano, Kazuo*; Koike, Masato
Spectrochimica Acta, Part B, 65(2), p.147 - 151, 2010/02
To meet the needs we have been developing an apparatus to evaluate polarization abilities of multilayer- and crystal-types polarizing elements and determine the polarization state of light in 1 keV region. The 8-axis goniometer called the polarization analysis-unit is equipped in this apparatus and consists of a phase shifter-unit and an analyzer-unit. All axes can be driven with HV compatible stepping motors. Both reflection- and transmission-types samples are available on P and A. Therefore, this apparatus makes it possible to carry out not only conventional reflection and transmission measurements but also four scanning modes which are double- reflections and transmissions, and transmission-reflection and vice versa.
Koike, Masato; Ishino, Masahiko; Imazono, Takashi; Sano, Kazuo*; Sasai, Hiroyuki*; Hatayama, Masatoshi*; Takenaka, Hisataka*; Heimann, P. A.*; Gullikson, E. M.*
Spectrochimica Acta, Part B, 64(8), p.756 - 760, 2009/08
W/C and Co/SiO multilayer laminar-type holographic plane gratings (groove density 1/1200 lines /mm) in the 1-8 keV region are developed. For the Co/SiO grating the diffraction efficiencies of 0.41 and 0.47 at 4 and 6 keV, respectively, and for the W/C grating 0.38 at 8 keV are observed. Taking advantage of the outstanding high diffraction efficiencies into practical soft X-ray spectrographs a Mo/SiO multilayer varied-line-spacing (VLS) laminar-type spherical grating (1/2400 lines /mm) is also developed for use with a flat field spectrograph in the region of 1.7 keV. For the Mo/SiO multilayer grating the diffraction efficiencies of 0.05-0.20 at 0.9-1.8 keV are observed. The FWHM's of the measured line profiles of Hf-M (1644.6 eV), Si-K (1740.0 eV),and W-M (1775.4 eV) are 13.7 eV, 8.0 eV, and 8.7 eV, respectively. It shows the validity of multilayer lamina-type gratings in the region.
Shinonaga, Taeko*; Esaka, Fumitaka; Magara, Masaaki; Klose, D.*; Donohue, D.*
Spectrochimica Acta, Part B, 63(11), p.1324 - 1328, 2008/11
The isotopic composition of single uranium and plutonium particles was measured with an inductively coupled plasma mass spectrometer (ICP-MS) and a thermal ionization mass spectrometer (TIMS). The particles prepared on a carbon planchet were first analyzed with an energy dispersive X-ray spectrometer (EDX) attached to a scanning electron microscope (SEM) and then transferred on to a silicon wafer using a manipulator. The particle on the silicon wafer was dissolved with nitric acid and the isotopic ratios of U and Pu were measured with ICP-MS and TIMS. The results obtained by both methods showed good agreement with the certified values within the expected uncertainty. The measurement uncertainties obtained in this study were similar for both mass spectrometric methods. This study was performed to establish the method of particle analysis with SEM, EDX, the particle manipulation technique, and the measurement of isotope ratios of U and Pu in a single particle by mass spectrometry.
Zhang, X. Z.*; Esaka, Fumitaka; Esaka, Konomi; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu; Watanabe, Kazuo
Spectrochimica Acta, Part B, 62(10), p.1130 - 1134, 2007/10
The capability of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of uranium isotope ratios in individual particles was determined. For this purpose, we developed an experimental procedure including single particle transfer with a manipulator, chemical dissolution and isotope ratio analysis. As the result, the U/U isotope ratio for the particle with the diameter between 0.5 and 3.9 m was successfully determined with the deviation from the certified ratio within 1.8%. The developed procedure was successfully applied to the analysis of a simulated environmental sample prepared from a mixture of indoor dust (NIST SRM 2583) and uranium particles (NBL CRM U050, U350 and U950a). From the results, the proposed procedure was found to be an alternative analytical tool for nuclear safeguards.
Muramatsu, Yasuji; Yamashita, Michiru*; Motoyama, Muneyuki*; Denlinger, J. D.*; Gullikson, E. M.*; Perera, R. C. C.*
Spectrochimica Acta, Part B, 59(8), p.1317 - 1322, 2004/08
Polarized emission spectra from graphite have been measured by an EPMA and discussed by means of molecular orbital calculation of 2p electrons densities of state of graphite by some of the present authors. The present study treats the refined measurements of the polarized C K-emission band spectra from the highly oriented pyrolytic graphite (HOPG) and discusses the structure of the surface carbons of Japanese traditional smoked roof tiles, Ibushi Kawara.
Esaka, Fumitaka; Watanabe, Kazuo; Onodera, Takashi; Taguchi, Takuji; Magara, Masaaki; Usuda, Shigekazu
Spectrochimica Acta, Part B, 58(12), p.2145 - 2155, 2003/12
In order to improve the sensitivity of elemental analysis for aerosol particles by total-reflection X-ray fluorescence spectrometry (TXRF), silicon wafer carriers with diameters of 25 mm were selected and prepared for direct impact collection and subsequent analysis. The detection limits of elements on the carrier were determined and found to be superior to those on glassy carbon and quartz glass carriers used in previous studies. By using the silicon wafer carriers, aerosol particles with the sizes of 2.0 m, 0.3-2.0 m and 0.05-0.3 m were collected at Ibaraki in Japan from January to August 2002 and analyzed by TXRF. Selenium Consequently, the elements with the concentration of ng/m &8211; pg/m in the particles were successfully detected. The results revealed that K, V, Zn, Br and Pb were concentrated in fine particles, which is presumed to arise from anthropogenic sources. In contrast, Ca, Ti and Fe were contained in coarse particles, which is presumed to arise from soil.
Spectrochimica Acta, Part B, 39(8), p.979 - 991, 1984/00
no abstracts in English
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Spectrochimica Acta, Part B, 36(7), p.687 - 695, 1981/00
no abstracts in English