Advances in X-Ray Chemical Analysis, Japan
Online ISSN : 2758-3651
Print ISSN : 0911-7806
Volume 42
Displaying 1-40 of 40 articles from this issue
Review Articles
  • Akihide DOSHO, Koichi ISHIBASHI
    2011 Volume 42 Pages 7-15
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    X-ray diffraction quantitative analyses are discussed for samples on filter. In general quantitative analysis with the calibration curve is used for filter sample. But there is a quantitative analysis without calibration curve, which is relatively easy method because it is unnecessary to provide any calibration curve. The relative intensity of the crystallites on filter is measured against pure polycrystalline material. The relative intensity with the absorption correction becomes weight ratio of the crystallites on filter. These two methods are quantitative based on the intensity corrected absorption data.

    Download PDF (4323K)
  • Hiromi EBA, Toru TAKAYAMA, Hirohisa NAGATANI, Kazuhiko NAKANO, Hisashi ...
    2011 Volume 42 Pages 17-43
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    In this article, the interesting X-ray analysis-related literatures, which are published on academic journals during the year 2010, are summarized. The number of the researched journals is 19, including two Japanese journals, which contribute the advance of the X-ray analysis in the field not only of analytical chemistry but also of spectroscopy and physics. In every journal, the trend of the X-ray analysis methods and of the measured specimens, the topics of analytical technique and of the developed components of the X-ray analysis apparatus, and the comments for the nortable articles are mentioned. The constitution and revision of standards of X-ray analysis on Japanease Industrial Standard (JIS) are shown. The websites of the company related with X-ray tools or X-ray apparatus are also shown, and the information on technical reports is available.

    Download PDF (11570K)
  • Takayuki SHIOSE
    2011 Volume 42 Pages 45-52
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    We report holding a special exhibition on X-ray researches at the Kyoto University Museum, 2010 spring-summer. At the exhibition, we show X-ray photographs of various objects, such as humans, animals, robots, cultural properties, and a supernova explosion. We will also exhibit X-ray apparatus that were used in the earliest days of the X-ray research in Japan to show history of X-ray research. Even today, more than 100 years after X-ray was discovered, X-ray technology is still very important in many fields.

    However, many people often misunderstand it. For example, some patients refuse to have X-ray examination because they are too afraid of an effect of radioactive ray. Our aim is to promote correct understanding of X-ray technology by showing what appear and what do not appear in a X-ray photograph.

    Download PDF (5561K)
  • Shinya FUJIMOTO
    2011 Volume 42 Pages 53-58
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Recent advanced Backscatter Imaging technology to highlight organic threats and contraband that conventional transmitting X-ray systems miss — explosives, plastic weapons, and drugs. Principles of backscatter imaging system and comparison of explosive detection performance between backscattered X-ray images and transmitted X-ray images are briefly described.

    Download PDF (5693K)
  • Shinsuke KUNIMURA
    2011 Volume 42 Pages 59-74
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Total reflection X-ray fluorescence (TXRF) spectrometry was first proposed by Yoneda and Horiuchi in 1971, and this spectrometric method has been applied to various fields such as semiconductor analysis and environmental analysis since 1971. In the present review, the following points are introduced: (1) How TXRF analysis improves detection sensitivity; (2) Development and features of various types of TXRF spectrometers such as a portable spectrometer; (3) Features of X-ray optics.

    Download PDF (8023K)
  • Jun KAWAI
    2011 Volume 42 Pages 75-82
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Physical meaning of X-ray total reflection, which has been erroneously explained in a text book of Waseda and Matsubara, is explained through the way of Feynman's path integrals. The total reflection of X-rays is the result of the sum of the possible all paths including the phase. Consequently the total reflection is the same as the Bragg diffraction. The relation between the reflectivity curve and dynamical theory of X-ray diffraction is explained after Takahashi and Nakatani. Egorov's X-ray wave guide and related techniques, which use the X-ray total reflection phenomena, are also described.

    Download PDF (4119K)
  • Hidekazu TAKANO
    2011 Volume 42 Pages 83-94
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    X-ray focusing techniques are rapidly improving especially in the hard X-ray region with the development of synchrotron radiation sources and high precision fabrication techniques. However, in Fresnel zone plates and Kirkpatrick-Baez (KB) mirors which have been used as the general device for X-ray focusing, the focusing performance nowadays is close to their theoretical limits. By advent of new focusing devices, such as multilayer Laue lenses and graded multilayer KB mirrors, to overcome the limits, the best X-ray focus size becomes around 10 nm. And an X-ray focusing beam, called as “microbeam” in several years ago, is now called as “nanobeam”.

    In this review, basis of focusing optics and X-ray focusing devices generally used are first described. Then new focusing devices and present status of X-ray nanofocusing are introduced, and future of X-ray focusing is mentioned.

    Download PDF (6497K)
  • Hidenori TOYOKAWA
    2011 Volume 42 Pages 95-110
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Photon counting method is a standard X-ray analysis technique, especially for energy-resolved or wide dynamic-range measurements. 1D or 2D photon counting array detectors have been developed recently and made extremely advanced analysis possible in synchrotron radiation experiments. In particular, the PILATUS detectors developed by the PSI represent the world largest single photon counting 2D-detector and overcome the existing imaging plate and CCD detector's limitations such as a slow readout time. SPring-8 has closely collaborated in the PILATUS project since the early stage. This paper describes the PILATUS detector and its applications at SPring-8 firstly, and then reports the other counting-type 1D and 2D detector developments.

    Download PDF (8944K)
Original Papers
  • Long ZE, Yasukazu NAKAYE, Yusuke MORIKAWA, Jun KAWAI
    2011 Volume 42 Pages 111-114
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Silicon drift detector (SDD) is recently used in a scanning electron microscope. In X-ray measurement using an SDD, black-box digital signal processor is usually used. However, by using a musician's audio amplifier and self-programmed signal processing, the SEM-EDX measurement is possible.

    Download PDF (2371K)
  • Hiroki NAGAI, Yoshihide NAKAJIMA, Shinsuke KUNIMURA, Jun KAWAI
    2011 Volume 42 Pages 115-123
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    We have adapted a silicon drift detector (SDD) to a portable total reflection X-ray fluorescence (TXRF) spectrometer using polychromatic X-rays from an X-ray source of single-digit watt. Analytical performance was greatly improved in PB ratio and the sensitivity for lighter elements when compared with the former spectrometer equipped with a Si-PIN detector.

    In this article improved sensitivity of the new spectrometer is described, and additionally the evaluation of the current wave-guide, a newly developed sample preparation device for precise quantitative evaluation and an application to the analysis of suspended particles are reported.

    Download PDF (4603K)
  • Akihiko IWATA, Jun KAWAI
    2011 Volume 42 Pages 125-139
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Many of Bi-colour coins which composed two different colour alloys have similar colour and feel of materials, and are considered to use similar alloys. Typical Bi-colour coin, EUR coins, are produced in different countries independently but based on the same EU regulations, its composition of elements are regulated by the regulations.

    Nowadays identification of type of metal and alloy is easy and quick work, since hand-held ED-XRF systems have been widely used. However identification of production county of same type of alloy has not been attempted. We report the trial result of identification of production county using similar Bi-colour coins including EUR coins which produced in different countries and based on same the regulations.

    Download PDF (7066K)
  • Tsutomu NAGAYOSHI, Takeyoshi TAGUCHI, Toru TANIMORI, Hidetoshi KUBO, J ...
    2011 Volume 42 Pages 141-152
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    The micro-pattern gas detector (MPGD) has a fine electrode structure, and it can obtain much higher positional resolution compared to that of the conventional gas detector based on the multi-wire proportional chamber. The “Micro Pixel Chamber (μ-PIC)” is a new MPGD developed at Kyoto University. It has been applied not only to X-ray crystallographic analysis, but also particle and nuclear physics. In the present study, some experiments were conducted in order to evaluate the capability of μ-PIC in X-ray analysis. The gas gain of 3000 and linearity up to 200 kcps were obtained. Effect of parallax was examined, showing the image distortion within the theoretical estimate. Small angle X-ray scattering experiment using a collagen sample was also conducted, having demonstrated good X-ray imaging performance of μ-PIC.

    Download PDF (5904K)
  • Katsumi MARUMO, Yuka ONOKI, Harumi OHTSUKA, Yoshinori HOSOKAWA
    2011 Volume 42 Pages 153-165
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    We developed a transmission X-ray fluorescence spectrometer (TXRF) combining an X-ray CCD camera and an energy dispersive X-ray fluorescence (EDXRF) analytical system, in order to provide a new tool for risk assessment of toxic metals (e.g. arsenic and lead) in contaminated soils. Assuming the thickness of soil grains are proportional to their mean diameters, it is possible to distinguish low density soil grain (e.g. quartz) from high density soil grain (e.g. lead-bearing minerals) of same mean diameter, by changing X-ray tube voltage and monitoring the gray level (brightness) of the X-ray image of these soil grains. This transmission X-ray imaging technique of TXRF was applied to determine the density of soil grains of lead-bearing artificial contaminated soils, as well as soil grains of arsenic-bearing contaminated soils caused by natural origin.

    The TXRF study suggests that the lead in the contaminated soil with high lead leachability (lead concentration and leachability are 15,000 mg/kg and 4,800 μg/L, respectively) contains a soil grain showing characteristic X-rays of manganese, iron, copper, zinc and lead. X-ray transmission image of the soil grain changes from dark to pale and finally the image disappear before X-ray tube voltage run up to 50 kV, suggesting that the grain is not a high density material. We assume that lead, copper and zinc of the grains occur as the absorbed phase on manganese minerals (e.g. manganese oxide and/or hydroxide) which can release lead during the leaching test.

    Meanwhile, the lead in the contaminated soil with low lead leachability (lead concentration and leachability are 6,900 mg/kg and 3.5 μg/L, respectively) contains a soil grain showing the strong characteristic X-rays of lead. The lead-bearing soil grain remains its X-ray transmission image even at the maximum X-ray tube voltage (50 kV), suggesting the grain is high density material as lead compounds (e.g. lead sulfide and lead carbonate).

    Using the XRF data and the relationship between grain sizes and their gray levels, the TXRF study of arsenic contaminated site suggests that the arsenic in the contaminated soil with high arsenic leachability (arsenic concentration and leachability are 210 mg/kg and 41 μg/L, respectively) occurs as arsenic sulfide, meanwhile, the arsenic in the contaminated soil with low arsenic leachability (arsenic concentration and leachability are 210 mg/kg and 5 μg/L, respectively) occurs as secondary iron minerals. The TXRF and XRD data suggest that the secondary iron mineral is the sulfate-bearing iron-oxyhydroxide schwertmannite (Fe8O8(OH)6-2x(SO4)x), which can fix arsenic for sulfur site and prevent releasing of arsenic during the leaching test.

    Download PDF (6650K)
  • Yoshie ARAKI, Hiroki YAMASHITA, Shinichi TERADA
    2011 Volume 42 Pages 167-173
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Peak deconvolution is necessary in elemental analyses by using X-ray spectrometry, in order to correct errors due to the overlapping of the emission peaks. In this report, we try to increase the accuracy to determine the compositions of samples by employing fundamental parameter (FP) method in the deconvolution process. The basic point is to determine default intra-element ratios by FP calculation. Since the ratios are dependent on composition of the sample as well as X-ray parameters such as tube voltage, anode material and the geometry of the spectrometer, we recalculate the ratios based on the composition that are calculated using default ratios. The peak intensities are refined when recalculated ratios are used. Calculated composition based on the refined intensities is also refined. Iterative calculations of peak deconvolutions and quantifications are also possible. We applied the refining method for various typical EDXRF applications that clearly show the effect and/or accuracy of ratios has strong effect in calculated peak intensities. In a spectrum of Cu-Zn alloy, Zn-Kα/Kβ ratio is strongly dependent on the composition since Zn-Kα is not strongly absorbed by Cu but Zn-Kα that has slightly higher energy than Cu-K absorption edge. A similar example is Ag-Pd alloy. Pd-K absorption edge is between Ag-Kα and Ag-Kβ Ratios of L-lines are more dependent on the composition in many cases since absorption of irradiating X-rays and secondary excitation also affect the ratios. Examples of a gold alloys are shown. Trace Pb, Bi, As analysis in Sn based alloy is a good example of the effect of the refinement. If we use the ratios that are experimentally determined on single element metal reference, peak deconvolution results zero intensity of As-Kα On the other hand, if we refine the ratios using FP method, better fitting is achieved and As-K line intensity is calculated properly.

    Download PDF (4384K)
  • Minoru INOUE, Yasujiro YAMADA, Mao KITAMURA, Norifumi GOTOH
    2011 Volume 42 Pages 175-181
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    In quantitative analysis of components in quicklime using WDXRF, we studied optimum measuring conditions for the analysis of carbon dioxide in pressed pellet method. We also studied the analysis of loss on ignition in the quicklime and could obtain adequate accuracy in practical analysis by using the intensities of Compton scattering X-rays. Additionally it was found that matrix correction of coexisting components is effective in the analysis of loss on ignition.

    Download PDF (3788K)
  • Yoshihiro OKAMOTO, Hideaki SHIWAKU, Shinichi SUZUKI, Tsuyoshi YAITA
    2011 Volume 42 Pages 183-195
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    X-ray imaging technique was used to add position sensitivity to XAFS measurement technique. Only the ionic chamber at the downstream of the sample is replaced by an X-ray CCD camera. X-ray intensity is obtained by digitalizing 8-bit gray scales of pictures from the CCD camera. The EXAFS curve fitting analyses of some standard samples like Cu foil show that the imaging XAFS is qualitatively enough though there are some limitations in quantitative analysis such as coordination number. It was confirmed from analysis of the mixture sample that the position sensitivity was successfully added to the XAFS technique.

    Download PDF (6783K)
  • Hisashi HAYASHI, Toshimi AOKI, Atsuko OGAWA, Sayo OMURA, Noriko KANAI, ...
    2011 Volume 42 Pages 197-206
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Kβ fluorescence spectra of the metal oxides, TiO2, V2O5, Fe2O3/SiO2, which were formed in sol-gel processes, have been measured by using a wavelength-dispersive type X-ray spectrometer. While the spectra observed after the calcinations were little different from those of standard samples, the wet gels and dry gels brought noticeable intensity change (∼10%) in the Kβ' and Kβ” region. In the Fe2O3/SiO2 system, the preparation conditions of the sols can influence the Kβ' intensity, when the Fe concentrations are less than ∼2 mol %. The applicability of the Kβ satellite spectra to the characterization of the oxide gels is discussed.

    Download PDF (5124K)
  • Hideki YAMAMOTO, Masaaki HARADA
    2011 Volume 42 Pages 207-212
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    The agar electrolyte after electrolysis was observed by X-ray fluorescence imaging, and it was found that the metal ions eluted from the anode were accumulated at a constant distance from it. To investigate this phenomenon, the agar electrolyte was electrolyzed under several conditions and observed by X-ray fluorescence imaging, and diffusion rates of metal ions in the agar electrolyte were estimated.

    Download PDF (3342K)
  • Motoki IWASE, Yuki FUJIO, Shun NAGAHAMA, Keiji YAMADA, Tsutomu KURISAK ...
    2011 Volume 42 Pages 213-219
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Preparing phosphorus-doped TiO2 (P-TiO2) using phosphide as a precursor of P was attempted as a new method. P-TiO2 was obtained by the calcination after grinding phosphide and TiO2 materials in a mortar. The synthesized P-TiO2 nanoparticles exhibited a light yellow color or a gray color. The UV-vis diffuse reflection spectra of P-TiO2 showed a continuous absorption in the visible region. The photodegradation amount of phenol in the presence of P-TiO2 under UV light irradiation was larger than that in the presence of ST01. XRD patterns of P-TiO2 showed the presence of anatase. XPS spectra of P-TiO2 showed a P 2p binding energy around 134 eV, which indicated that P was incorporated into the titanium oxides. We discuss a correlation between the features found by X-ray spectroscopic characterization and the photocatalytic activity.

    Download PDF (3468K)
  • Yoshitoki IIJIMA, Mikio NARUSE, Yuji SAKAI, Kenzo HIRAOKA
    2011 Volume 42 Pages 221-228
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Depth profiling analysis with X-ray photoelectron spectroscopy was performed on the surface of PET, PS, PMMA and PVC etched by charged water drople ([(H2O)90,000+100H]100+) impact (EDI). Even after prolonged irradiation with charged water droplets as long as 120 min, no change in the XPS spectra and substantial increase in surface roughness in the AFM images of these polymers were observed. The etching mechanism due to EDI can be estimated as follows, the main chain unit of polymers was etched without damage. The EDI etching was proved to be a useful method for XPS depth profiling of polymer materials.

    Download PDF (4487K)
  • Tomohiro MATSUSHIMA, Yukio USUI
    2011 Volume 42 Pages 229-235
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    In order to accurately and quantitatively evaluate internal center segregation in slabs and thick steel plates, quantitative mapping of Mn has been investigated by the calibration curve method of Electron Probe Micro Analyzer. Fe-Mn binary alloys with almost uniform distribution of Mn, in which the precipitate-forming elements of C and S are reduced, has been fabricated and the accuracy (σd) of the calibration curve has been evaluated. The accuracy of 0.004 mass % was obtained by point analysis of the binary alloys, which is better than that of 0.010 mass % obtained by area analysis of Standard Reference Material (SRM). The measurement time taken to create the calibration curve was significantly reduced from 200 seconds for area analysis of the SRM to 25 seconds for point analysis of the binary alloys. The solidification structure in a laboratory sized ingot that contains 1.9 mass % Mn has been evaluated and the variation of the area that contains more than 2.2 mass % Mn in three time measurements was reduced from 2.0 % by area analysis of the SRM to 0.5 % by point analysis of the binary alloys.

    Download PDF (4003K)
  • Takashi YAMAMOTO, Makoto KIKUCHI, Saki OKADA, Kazuhide YAMASHITA, Chis ...
    2011 Volume 42 Pages 237-248
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Iron ion-promoted silica solid acid catalysts active for α-methylstyrene dimerization were characterized by XRD and Fe K-edge XANES/EXAFS spectroscopic techniques. The possible active species were proposed. The 1 mol % of iron to Si was incorporated in catalyst samples, which was prepared by sol-gel process using iron chloride and tetraethylorthsilicate (TEOS) as the sources. The incorporated trivalent iron species were characterized as tetrahedral FeOxCl4-x, and excess loaded species were aggregated to form α-Fe2O3 during drying process at 403 K. The fraction of [FeOxCl4-x], [FeCl6] and [FeO6] species in the catalyst samples were determined by the least-squares analysis of XANES.

    Download PDF (6372K)
  • Yasukazu NAKAYE, Jun KAWAI
    2011 Volume 42 Pages 249-253
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Pyroelectric-type X-ray tube works only with a 9 V buttery and used as an X-ray source for portable X-ray fluorescence measurement. However, it has a problem with its unstable tube current. The present work is to investigate the possibility of the tube current control of the Pyroelectric-type X-ray tube. Ion current and electron beam current are measured on changing the temperature of the LiTaO3 crystal on which a tungsten tip was fixed. Novel phenomenon is observed that field emission driven by the LiTaO3 crystal becomes a pulsed emission.

    Download PDF (4678K)
  • Yasukazu NAKAYE, Jun KAWAI
    2011 Volume 42 Pages 255-259
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    We utilized an audio digitizer in EDXRF with a CdTe detector and an SDD detector. With an electromagnetic shielded audio digitizer, more than 3 times higher energy resolution was achieved compared with the audio digitizer on the computer main board, because of the absence of the circuit noise.

    Download PDF (3513K)
  • Deh Ping TEE, Jun KAWAI
    2011 Volume 42 Pages 261-266
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    A portable total reflection X-ray fluorescence spectrometer was applied to 5 commercial bottled mineral water and a tap water which from different countries. Six dry residues, prepared by pipetted a 10 μL portion of each bottled drinking mineral water on sample holder. The certified concentrations on the bottle label of the commercial bottled mineral waters are ranged from several tens of ppb to several hundreds ppm. Calcium, potassium, or vanadium contained in the commercial bottled water was easily detected. Potassium, calcium, chlorine, and zinc were detected in the tap water. This kind of small and highly sensitive spectrometer is feasible to be used for the rapid monitoring of elements in the spring or tap water before an accurate and precise analysis by tedious elemental analysis instruments.

    Download PDF (3052K)
  • Yasuji MURAMATSU, Eric M. GULLIKSON
    2011 Volume 42 Pages 267-272
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    To obtain the standard XANES in the CK region of highly oriented pyrolytic graphite (HOPG), carbon nanotube (CNT), and carbon black (CB), high-resolution CK-XANES of them were measured under the magic angle of the incident angle. The magic angle was measured as 55° from the comparison of their incident-angle-dependent CK-XANES. In the CK-XANES measurements under the magic angle, HOPG, CNT, and CB take a similar π** peak height ratio, which shows that they are composed of hexagonal carbon layers. The π* peak width and the spectral profile in the π** region of CNT and CB are different from those of HOPG, which suggests that the electronic structures in the π orbitals of CNT and CB are different from HOPG.

    Download PDF (3787K)
  • Yasuji MURAMATSU, Yuki KUBOTA, Sachiyo TAMAYA, Eric M. GULLIKSON
    2011 Volume 42 Pages 273-280
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    X-ray absorption near-edge structure (XANES) in the CK and OK regions of the liquid organic compounds such as Isoprene, 2,6-dimethyl-2,4,6-octatriene, Geraniol, Farnesol, Squalene, Geranylacetone, (-)-Citronellal, Hexadecylbenzene, and Epoxy resin can be directly measured in a vacuum measurement chamber. The liquid samples were coated on indium substrates, and the XANES measurements were performed using a total-electron-yield (TEY) method. The successfully-measured TEY-XANES shows that the direct measurements of liquid compounds coated on indium substrates are useful to easily obtain the XANES without a liquid cell.

    Download PDF (4835K)
  • Tsutomu KURISAKI, Yusuke MIKI, Keita MINAMI, Syohei YOKOYAMA, Shinichi ...
    2011 Volume 42 Pages 281-290
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    We developed two new soft X-ray absorption spectrometers: one is a laboratory scale ultra soft X-ray absorption(USXA) spectrometer for measuring ultra soft X-ray absorption spectra (50-150 eV) of solid samples such as battery materials, soil and rock and the other is a soft X-ray absorption spectrometric apparatus for measuring soft X-ray absorption spectra (50-1500 eV) of solution samples such as electrolyte solution, wet soil, and living specimen of animals and plants at the BL-12 of Kyushu Synchrotron Light Research Center, Japan. The former spectrometer consists of four sub-systems: (i) a laser and focusing optics; (ii) target and target chamber; (iii) monochromator; and (iv) detector system and sample chamber. We examine the Li-K XANES spectral measurements of lithium halides using the USXA spectrometer. The latter spectrometer has 7 kinds of movable axes and enables to perform the soft X-ray absorption measurements with a fluorescent mode under atmospheric pressure. We carried out the measurements of soft X-ray absorption spectra for varying concentration in aqueous solutions of sodium chloride and magnesium chloride. The obtained experimental XANES spectra are analyzed using the theoretically calculated spectra from the DV-Xα method.

    Download PDF (4735K)
  • Hisashi HAYASHI, Eriko GOH, Yuri HIROSE
    2011 Volume 42 Pages 291-297
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    X-ray beams of Cu Kα with the size of 0.3 × 1 mm2 were irradiated on the leaves of two kinds of water plants, Eichhornia crassipes and Egeria densa, to measure their X-ray fluorescence (XRF) spectra. Under in-vivo conditions, the XRF spectra of the two plants showed no marked change with passage of time. On the other hands, for their cut leaves, the intensity of Ca Kα (in some case, K Kα, Mn Kα, and Fe Kα also) clearly increased over a period of 1∼3 hours. Damages of ion control systems in the plants were suggested as a possible reason of this curious cutting effects.

    Download PDF (4137K)
  • Koichi MURAOKA, Masahiro AWAZU, Tadashi UTAKA, Kazuo TANIGUCHI
    2011 Volume 42 Pages 299-306
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    An energy dispersive X-ray fluorescence analyzer has been used to screen the hazardous heavy elements as a non-destructive manner with rapid and high reproducibility. On the other hand, with the increasing wide varieties of measuring samples, more sensitivity of lower limits of detection has been requested. To satisfy these demands, we have developed a portable and resource-saving EDX analyzer using a miniature X-ray tube of 50 W, an optical system with optimized primary beam filter and a portable semiconductor detector with Peltier cooling system. In this study, based on the measurement data obtained by sensitive quantitation of cadmium in rice that is catching public attention, we emphasize the approach to the management system of cadmium concentration. And regarding detector of hard X-ray element by this instrument, we also introduce some X-ray optical technologies and hardware configurations.

    Download PDF (4065K)
  • Yasuji MURAMATSU, Tsuyoshi OE, Rie OGAWA, Makoto NISHINO, Hitomi OHNO, ...
    2011 Volume 42 Pages 307-313
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    To clarify the magnetization of the old coin, Kan'ei Tsuho, distributions of metal elements (Cu, Zn, Fe, S, Cl, Pb, As, Ca) were analyzed by fluorescent X-ray spectroscopy. It can be confirmed that the measured Kan'ei Tsuho samples were made of brass (Cu-Zn alloy). Although concentrations of impurity Fe and S were different among the samples, definite relationship between the magnetization and concentration of Fe can not be observed. This suggests that magnetization of Kan'ei Tsuho can not be explained from the distribution of Fe.

    Download PDF (4714K)
  • Rie OGAWA, Hirotomo OCHI, Makoto NISHINO, Naoto ICHIMARU, Ryosuke YAMA ...
    2011 Volume 42 Pages 315-324
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Quantitative analysis of small quantities of organic samples was performed by X-ray fluorescence analysis using the fundamental parameter method. Intensity ratio calculations with respect to fluorescent X-rays using continuous scattered X-rays and quantification of the hydrocarbon (principal component of the samples) using Rh Kα Compton scattered X-rays were investigated for shape correction. The results indicated that continuous scattered X-rays are suitable for low-concentration samples, such as foods, and Rh Kα Compton scattered X-rays are suitable for high-concentration samples, such as polyvinyl chloride resin. It was also shown that which method to use can be determined using a threshold value for the measured intensity ratios calculated using Rh Kα Compton scattered X-rays and Rh Kα Rayleigh scattered X-rays.

    Further investigations indicated that the intensity ratio of the Rh Kα Compton scattered X-rays and Rh Kα Rayleigh scattered X-rays can be used for shape correction, as well as to differentiate between the methods described above. This method may result in some discrepancies in the quantitation values, but is expected to be effective for the analysis of small quantities of both high-concentration and low-concentration organic samples.

    Download PDF (4753K)
  • Hiroshi GONDAI, Yoshinari ABE, Izumi NAKAI
    2011 Volume 42 Pages 325-340
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Among archaeological artifacts of glass and glazed pottery, there is a particular type that contains high levels of heavy elements, such as lead and tin. Though XRF is a well-established analytical method and is suitable for analysis of archaeological objects because of the nondestructive multi-element analytical capability and its rapid and easy operation of the instrument, it is difficult to perform quantitative analysis of the samples containing high level of heavy elements like Pb due to the matrix absorption effect. In this paper, we attempted to look for the correction model, which can provide improved calibration curves from the perspective of empirical correction method. We have proposed a new correction model, which was derived by regression analysis using analytical data of inhouse standard specimens prepared by mixing oxide or carbonates of the component elements. This model formula involved two important variables, PbO and SnO2 contents.

    When we prepared the calibration curves based on our correction model, their linearity has improved spectacularly. This analytical method was successfully applied to the archaeological characterization of Islamic luster-painted pottery excavated from Raya site, Sinai, Egypt, where we carried out XRF analysis by using portable XRF instrument. It is expected that this method can be utilized widely for quantitative chemical analysis of the lead containing glaze and glass by using XRF analysis.

    Download PDF (7202K)
  • Shinjiro HAYAKAWA, Haruna TABATA, Tatsuya SHIMAMOTO, Satomi MORI, Take ...
    2011 Volume 42 Pages 341-346
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Gold thin film deposited onto a thin Kapton film was utilized as a working electrode in an electrochemical cell for X-ray fluorescence analysis. In-situ measurement of Cu plating was carried out, and the evaluated film thickness from the X-ray fluorescence spectrum was almost identical to that obtained from the electrochemical measurements. The present detection limit with the sealed X-ray tube was 0.3 nm in Cu thickness, and the use of the small working electrode will reduce the detectable amount down to 20 ng.

    Download PDF (3168K)
  • Yuichi YOSHII, Akiko HOKURA, Tomoko ABE, Misao ITOUGA, Hitoshi SAKAKIB ...
    2011 Volume 42 Pages 347-358
    Published: March 31, 2011
    Released on J-STAGE: November 29, 2023
    JOURNAL FREE ACCESS

    Scopelophila cataractae is known as a “copper moss”. It is known as a peculiar moss which can accumulate high level of metals (Cu, Pb, etc.) in its plant body. This moss is expected as a material to collect metals from water. In this study, gametophyte's leaf of the moss was examined by μ-XRF imaging, and Cu K-edge and Pb L1-, L3-edge XAFS analyses to reveal the accumulation behavior of Cu and Pb. μ-XRF imaging was carried out utilizing X-ray microbeam at BL37XU, SPring-8 from the undulator source, and at BL-4A, Photon Factory KEK from the bending magnet. The results have revealed that Cu and Pb were accumulated on the cell wall of the leaf, and especially at the stereid cells of midrib. It was found that Cu-XANES spectra of the leaf were similar to that of copper(II) acetate, a reference substance. On the other hand, Pb XANES spectra of the leaf were similar to that of a reference, lead(II) stearate. These results suggested that these metals were bound to oxygen of carboxyl group in the plant. Consequently, it is assumed that Cu and Pb could be bound to acidic sugar which is a component of its cell wall such as pectic acid, polygalacturonic acid and others. Furthermore, to compare with other heavy-metal accumulating moss (Scopelophila ligulata and Sphagnum palustre), their gametophyte's leaves were also examined by μ-XRF imaging. S. ligulata accumulated Pb in its stereid cells of midlib, while S. palustre accumulated Pb in its hyaline cells.

    Download PDF (5940K)
Technical Notes
Conference Reports
feedback
Top