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Journal Articles

Unusually kinetically inert monocationic neptunyl complex with a fluorescein-modified 1,10-phenanthroline-2,9-dicarboxylate ligand; Specific separation and detection in gel electrophoresis

Yamagata, Kazuhito*; Ouchi, Kazuki; Marumo, Kazuki*; Tasaki-Handa, Yuiko*; Haraga, Tomoko; Saito, Shingo*

Inorganic Chemistry, 62(2), p.730 - 738, 2023/01

 Times Cited Count:1 Percentile:81.75(Chemistry, Inorganic & Nuclear)

The inert NpO$$_{2}$$$$^{+}$$ complex with a fluorescein-modified phenanthroline-2,9-dicarboxylic acid was found by kinetic selection using polyacrylamide gel electrophoresis (PAGE) from a small chemical library. The small spontaneous dissociation rate constant of 8$$times$$10$$^{-6}$$ s$$^{-1}$$ (the half-life of 23 hours) was determined. This is the singly-charged NpO$$_{2}$$$$^{+}$$ complex exhibiting unusual kinetic inertness in aqueous solution, one million times slower than widely accepted fast kinetics of neptunyl complexes. Selective fluorescence detection of NpO$$_{2}$$$$^{+}$$ was achieved in PAGE with a detection limit of 68 pmol dm$$^{-3}$$(17 fg). This system was successfully applied to simulated spent nuclear fuel and high-level radioactive waste samples.

JAEA Reports

In-situ dismantling of the liquid waste storage tank LV-1 in the JRTF; The Dismantling work

Yokozuka, Yuta; Sunaoshi, Mizuho*; Sakai, Tatsuya; Fujikura, Toshiki; Handa, Yuichi; Muraguchi, Yoshinori; Mimura, Ryuji; Terunuma, Akihiro

JAEA-Technology 2021-037, 44 Pages, 2022/03

JAEA-Technology-2021-037.pdf:10.84MB

JAEA has dismantled equipment and instrument in the JAERI's Reprocessing Test Facility (JRTF) since 1996 as a part of its decommissioning. Starting in JFY 2007, in the annex building B which stored liquid waste generated in wet reprocessing tests, the liquid waste storage tank LV-1 installed in the LV-1 room of the first basement was dismantled with the in-situ dismantling method. The dismantling work is described in this report. Data on manpower, radiation control, and waste in the preparation work were collected, and its work efficiency was analyzed.

Journal Articles

Stoichiometry between humate unit molecules and metal ions in supramolecular assembly induced by Cu$$^{2+}$$ and Tb$$^{3+}$$ measured by gel electrophoresis techniques

Nakano, Sumika*; Marumo, Kazuki*; Kazami, Rintaro*; Saito, Takumi*; Haraga, Tomoko; Tasaki-Handa, Yuiko*; Saito, Shingo*

Environmental Science & Technology, 55(22), p.15172 - 15180, 2021/11

 Times Cited Count:4 Percentile:36.59(Engineering, Environmental)

Humic acid (HA) can strongly complex with metal ions to form a supramolecular assembly via coordination binding. However, determining the supramolecular size distribution and stoichiometry between small HA unit molecules constituting HA supramolecule and metal ions has proven to be challenging. Here, we investigated the changes in the size distributions of HAs induced by Cu$$^{2+}$$ and Tb$$^{3+}$$ ions using a unique polyacrylamide gel electrophoresis (PAGE) for the separation and quantification of HA complexes and metal ions bound, followed by UV-Vis spectroscopy and EEM-PARAFAC. It was found that the supramolecular behaviors of Cu$$^{2+}$$ and Tb$$^{3+}$$ complexes with HA collected from peat and deep groundwater (HHA) differed. Our results suggest that this supramolecular stoichiometry is related to the abundance of sulfur atoms in the elemental composition of HHA. Our results provide new insights into HA supramolecules formed via metal complexation.

JAEA Reports

In-situ dismantling of the liquid waste storage tank LV-1 in the JRTF; The Dismantling preparation work

Yokozuka, Yuta; Sunaoshi, Mizuho*; Fujikura, Toshiki; Suzuki, Shota; Muraguchi, Yoshinori; Handa, Yuichi; Mimura, Ryuji; Terunuma, Akihiro

JAEA-Technology 2020-017, 56 Pages, 2021/01

JAEA-Technology-2020-017.pdf:7.88MB

JAEA has dismantled equipment and instrument in the JAERI's Reprocessing Test Facility (JRTF) since 1996 as a part of its decommissioning. Starting in JFY 2007, in the annex building B which stored liquid waste generated in wet reprocessing tests, the liquid waste storage tank LV-1 installed in the LV-1 room of the first basement was dismantled with the in situ dismantling method. The dismantling preparation work is described in this report. Data on manpower, radiation control, and waste in the preparation work were collected, and its work efficiency was analyzed.

JAEA Reports

Maintenance of the Evaporator-II in Waste Treatment Facility No.2 (FY2015)

Handa, Yuichi; Nakajima, Ryota; Yonekawa, Akihisa*; Takatsu, Kazuki; Kinoshita, Junichi; Irie, Hirobumi; Suzuki, Hisao*

JAEA-Technology 2020-005, 22 Pages, 2020/06

JAEA-Technology-2020-005.pdf:6.43MB

The Evaporator-II is installed in Waste Treatment Facility No.2. The evaporator system treats intermediate level radioactive liquid waste for Nuclear Science Research Institute and more. It is maintenance the evaporator can once/3years by the maintenance plan. The evaporator can is important unit of the Evaporator-II system. This report summarizes record of maintenance the Evaporator-II in FY2015.

Journal Articles

A Suitable procedure for preparing of water samples used in radiocarbon intercomparison

Takahashi, Hiroshi*; Minami, Masayo*; Aramaki, Takafumi*; Handa, Hiroko*; Kokubu, Yoko; Ito, Shigeru*; Kumamoto, Yuichiro*

Radiocarbon, 61(6), p.1879 - 1887, 2019/12

 Times Cited Count:2 Percentile:11.91(Geochemistry & Geophysics)

Water sample for interlaboratory comparison (here after "comparison water") must have inalterable $$^{14}$$C concentration during the comparison campaign and inter-batches homogeneity. In this study, the procedure for preparing of comparison water was discussed. We employed that comparison waters were artificially made by mixing chemical reagents, controlling $$^{14}$$C concentration and chemical composition. We could prepare six comparison waters, having 1, 14, 37, 56, 72 and 100 pMC, respectively. The stable carbon isotopic values and chemical compositions of some batches were measured to exanimate the inter- batches homogeneity. The $$^{14}$$C discrepancies among the batches were negligible for the inter-laboratory comparison. Finally, the results of trial comparison in Japan will be presented. Most of $$^{14}$$C results of CO$$_{2}$$ extracted by six laboratories showed good agreements each other.

Journal Articles

Anomalous hall effect with giant hysteresis loop in La$$_{0.67}$$Sr$$_{0.33}$$MnO$$_3$$|SrRuO$$_3$$ superlattices

Shiomi, Yuki*; Handa, Yu*; Kikkawa, Takashi*; Saito, Eiji

Physical Review B, 92(2), p.024418_1 - 024418_4, 2015/07

 Times Cited Count:7 Percentile:35.75(Materials Science, Multidisciplinary)

Journal Articles

Transverse thermoelectric effect in La$$_{0.67}$$Sr$$_{0.33}$$MnO$$_3$$|SrRuO$$_3$$ superlattices

Shiomi, Yuki*; Handa, Yu*; Kikkawa, Takashi*; Saito, Eiji

Applied Physics Letters, 106(23), p.232403_1 - 232403_4, 2015/06

 Times Cited Count:28 Percentile:73.87(Physics, Applied)

Journal Articles

Spectral shape deformation in inverse spin Hall voltage in Y$$_3$$Fe$$_5$$O$$_{12}|$$Pt bilayers at high microwave power levels

Lustikova, J.*; Shiomi, Yuki*; Handa, Yu*; Saito, Eiji

Journal of Applied Physics, 117(7), p.073901_1 - 073901_7, 2015/02

 Times Cited Count:7 Percentile:31.13(Physics, Applied)

Journal Articles

Present state of TEM-SXES analysis and its application to SEM aiming chemical analysis of bulk materials

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.682 - 683, 2014/08

X-rays originate form electronic transitions from valence bands (VB, bonding electron states) to inner-shell electron levels inform us energy states of bonding electrons. We have developed the SXES spectrometers attaching to TEM, EPMA, and SEM. A spectrometer has an energy range of 50-4000 eV by using four varied-line-spacing gratings. Applications of TEM-SXES instrument to C$$_{60}$$ have revealed characteristic energy distribution of bonding electrons. Carbon K-emission spectra of C $$_{60}$$ crystals showed that both the peak structures in $$pi$$- and $$sigma$$-bands and the characteristic dip structure between the $$pi$$- and $$sigma$$-bonding states in monomer-C$$_{60}$$ disappear in the most polymerized-C$$_{60}$$ crystals. Bulk specimens were examined by applying SXES to a SEM. Al L-emission spectra of intermetallic compounds of Al$$_{2}$$Au, AlCo, and aluminum showed different intensity distributions due to different band structures originating from different crystal structures.

Journal Articles

Exciting possibilities of soft X-ray emission spectroscopy as chemical state analysis in EPMA and FESEM

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Terauchi, Masami*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.684 - 685, 2014/08

A novel wavelength dispersive soft X-ray emission spectrometer (SXES) having a X-ray energy range of 50-210 eV has been developed. One feature is that the SXES is parallel detection of the signals so that it can be used like a conventional energy dispersive spectrometer. The other is a high energy resolution, which is about 0.2 eV at Al-L comparable to those revealed by XPS and EELS. These features enable us to obtain meaningful information about chemical bonding in various bulk samples. The SXES can detect Li-K emission spectrum. In the case of an anode electrode of a lithium ion battery (LIB), two types of lithium peaks are observed: one lower energy peak at 50 eV and the other higher energy peak at 54 eV. It was found that the former peak corresponds to the amount of charging, whereas the latter corresponds to the metallic state of lithium.

Journal Articles

Chemical state information of bulk specimens obtained by SEM-based soft-X-ray emission spectrometry

Terauchi, Masami*; Koshiya, Shogo*; Sato, Futami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 20(3), p.692 - 697, 2014/06

 Times Cited Count:32 Percentile:91.15(Materials Science, Multidisciplinary)

Electron beam induced soft-X-ray emission spectroscopy (SXES) by using a grating spectrometer has been introduced to a conventional scanning electron microscope (SEM) for characterizing desired specimen areas of bulk materials. The spectrometer was designed as a grazing-incidence flat-field optics by using aberration corrected (varied-line-spacing) gratings and a multi-channel-plate detector combined with a charge-coupled-device camera, which has already applied for a transmission electron microscope. The best resolution was confirmed as 0.13 eV at Mg L-emission (50 eV), which value is comparable to that of recent dedicated electron energy-loss spectroscopy instruments. This SXES-SEM instrument presents density of states of simple metals of bulk Mg and Li. Apparent band structure effects have been observed in Si L-emission of Si-wafer, P L-emission of GaP-wafer, and Al L-emissions of intermetallic compounds of AlCo, AlPd, Al$$_{2}$$Pt, and Al$$_{2}$$Au.

Journal Articles

An Extension of detectable energy-range of SXES spectrometer for electron microscopes

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

JAEA-Conf 2013-001, p.77 - 80, 2013/09

We have been developing a soft X-ray emission spectroscopy (SXES) instrument for electron microscopes (TEM, EPMA/SEM) with an extension of detectable energy range to 50-4000 eV. An introduction of valence electron spectroscopy with microscopy will supply fruitful information on bonding electrons, which cannot be obtained by EELS and EDS. For extend the lowest (or highest) detection energy upto 50 eV (or 4000 eV), a new laminar-type varied-line-spacing (VLS) grating, JS50XL, (or JS4000) has designed and manufactured. JS50XL and JS4000 having 1200 and 2400 lines/mm as well as coated by Au and a new multilayer-structure of W/B$$_{4}$$C for a wide-band energy region of 2000-3800 eV, respectively. Those gratings were installed and tested in a SXES spectrometer attached to a TEM. The extension in lowest detection energy was confirmed by Mg-L emission (JS50XL). The energy resolution was 0.2 eV at Fermi edge of 49.5 eV. It can be also seen a sharp Fermi edge for Li-K emission spectrum of metal-Li. The high energy resolution was confirmed by Te-La emission at 3.8 keV (JS4000). The full width at half maximum of the peak was 27 eV. The detection energy range was successfully extended by using the two new VLS-gratings.

Journal Articles

Development and applications of a new soft X-ray emission spectrometer for electron probe microanalysis and/or nanoanalysis

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Terauchi, Masami*; Koeda, Masaru*; Nagano, Tetsuya*; et al.

JAEA-Conf 2013-001, p.13 - 15, 2013/09

A very unique high performance soft X-ray emission spectrometer (SXES) has successfully been developed which can be attached not only to transmission electron microscopes (TEMs), but also to scanning electron microscopes (SEMs) as well as electron probe microanalyzers (EPMAs). To extend the analyzed energy ranges, a newly designed laminar-type varied-line-spacing (VLS) grating JS50XL, for a lower energy range, 50-170 eV, and a multilayered VLS grating JS4000, for a higher energy range, 2000-4000 eV, have been developed and installed to this spectrometer. Application software has also been developed for a commercial use of SXES in several fields such as battery materials, steel and alloys, and electron devices. The appearance of this spectrometer attached to EPMA and a few results acquired are shown in the following figures. This development has been conducted as one of the projects of Collaborative Development of Innovative Seeds (Practicability verification stage) by Japan Science and Technology Agency.

Journal Articles

Development of an objective flat-field spectrograph for electron microscopic soft X-ray emission spectrometry in 50-4000 eV

Imazono, Takashi; Koike, Masato; Kawachi, Tetsuya; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; et al.

Proceedings of SPIE, Vol.8848, p.884812_1 - 884812_14, 2013/09

 Times Cited Count:7 Percentile:94.06

We have developed an objective soft X-ray flat-field spectrograph to be able to attach to electron microscopes. This spectrograph has two attractive features. One is that it is designed to cover a wide energy range of 50-4000 eV by using four varied-line-spacing holographic gratings optimized for 50-200 eV, 155-350 eV, 300-2200 eV, and 2000-4000 eV. They can be accommodated in the single spectrograph. The other is a newly invented W/B$$_4$$C multilayer coating covering the 2000-4000 eV range. It can enhance the diffraction efficiency above a practical level of $$sim1$$% at a constant incidence angle in the whole energy range.

Journal Articles

Chemical State Mapping via soft X-rays using a Wavelength Dispersive Soft X-ray Emission Spectrometer with High Energy Resolution

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Terauchi, Masami*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 19(Suppl.2), p.1258 - 1259, 2013/08

A new wavelength dispersive soft X-ray emission spectrometer (WD-SXES) consisting of newly developed diffraction gratings has been developed for soft X-ray emission spectroscopy. The WD-SXES with two types of diffraction gratings nominally covering an energy range between 50 and 210 eV has been installed to electron probe X-ray microanalyzers, JEOL JXA-8100, for commercial use. The energy resolution of this WD-SXES is nominally 0.3 eV, which is one order of magnitude better than that of conventional WDSs with layered dispersion elements. It is to be noted that the corresponding edge of Al$$_{2}$$B is shifted to higher energy side by about 1 eV. One of the energy range was selected from 72 to 73.5 eV whereas the other was from 73.5 to 75 eV. The contrast in the former map is reversed in the later map as expected even though the energy difference between two maps is only 1.5 eV. The study confirms the high potential for the characterization especially for chemical state mapping.

Journal Articles

Construction of a SXES spectrometer for a conventional SEM

Terauchi, Masami*; Koshiya, Shogo*; Sato, Futami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 19(Suppl.2), p.1278 - 1279, 2013/08

We have been developed and tested soft-X-ray emission spectroscopy (SXES) instruments by attaching to TEM and EPMA. The spectrometer has an energy range form 50-4000 eV by using four varied-line-spacing (aberration corrected) gratings. This SXES spectrometer inform us energy states of valence electrons (bonding electrons) form an identified specimen area by electron microscopy, which cannot be obtained by EELS and EDS. This provides not only the probing method for the energy states of valence electrons but also a sensitive tool for elemental and chemical identification. The spectrometer has applied also to a SEM (JEOL JSM-6480LV). As SEM can use a larger probe current and excitation volume of specimen than those of TEM, the detection time is about one order shorter than that of TEM. The energy resolution evaluated at AL-L$$_{3}$$edge is 0.16 eV. The spectrum of LaB$$_{6}$$ shows apparent intensity corresponds to B-K Fermi edge, showing chemical state of boron.

Journal Articles

A New grating X-ray spectrometer for 2-4 keV enabling a separate observation of In-L$$beta$$ and Sn-L$$alpha$$ emissions of indium tin oxide

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy, 62(3), p.391 - 395, 2013/06

 Times Cited Count:11 Percentile:59.64(Microscopy)

A new multilayer-coated varied line-spaced grating, JS4000, was fabricated and tested for extending the upper limit of a grating X-ray spectrometer for electron microscopy. This grating was designed for 2-3.8 keV at a grazing incidence angle of 1.35 deg. It was revealed that this new multilayer structure enables us to take soft-X-ray emission spectra continuously from 1.5 keV to 4 keV at the same optical setting. The full-width at half maximum of Te-L$$alpha$$$$_{1,2}$$ (3.8 keV) emission peak was 27 eV. Sn-L$$alpha$$ (3444 eV) and In-L$$beta$$$$_{1}$$ (3487 eV) peaks, which cannot be resolved by a widely used energy-dispersive X-ray spectrometer.

Journal Articles

Development of a flat-field spectrograph with a wide-band multilayer grating and prefocusing mirror covering 2-4 keV

Imazono, Takashi; Koike, Masato; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; Terauchi, Masami*; et al.

Journal of Physics; Conference Series, 425(15), p.152008_1 - 152008_4, 2013/03

 Times Cited Count:3 Percentile:79.71

We have developed a flat-field spectrograph equipped with a wide-band multilayer grating and prefocusing mirror for the 2-4 keV range. To realize a spectrograph without any mechanical movement, the multilayer has a newly invented layer structure to uniformly enhance the diffraction efficiency (or reflectivity) of the grating (or prefocusing mirror) at a fixed angle of incidence in the whole energy region. The multilayer structure consisting of W and B$$_4$$C layers has been deposited by ion beam sputtering method on a varied-line-spacing laminar-type holographic grating. Also the same multilayer has been done on a spherical substrate. The average diffraction efficiency (or reflectivity) of the multilayer grating (or spherical mirror) is in excess of 3% at 88.65$$^circ$$ (or 4% at 88.00$$^circ$$) in the 2.1-3.8 keV range. The throughput of the spectrograph with multilayer optics can be evaluated to be 2-5000 times higher than that with conventional optics coated by a gold layer.

Journal Articles

Development of a soft X-ray diffractometer for a wideband multilayer grating with a novel layer structure in the 2-4 keV range

Imazono, Takashi; Koike, Masato; Kawachi, Tetsuya; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; et al.

AIP Conference Proceedings 1465, p.33 - 37, 2012/07

 Times Cited Count:5 Percentile:85.25

103 (Records 1-20 displayed on this page)