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Volume 40, Issue 12
Displaying 1-11 of 11 articles from this issue
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Tadashi MOCHIZUKI, Akiko SAKASHITA, Yohichi ISHIBASHI, Naoki GUNJI, Hi ...1991 Volume 40 Issue 12 Pages 875-881
Published: December 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe characteristics for depth analysis by laser ablation/ICP-MS have been discussed. Parameters such as the magnitude of defocusing, laser power and pulse repetition rate, provided a great influence on the depth-resolution for the analysis of a tin-plated steel sheet. The use of a 10 mm-defocusing was effective to obtain high depth-resolution. The ablation rates were measured by observing cross sections of the craters obtained. Remarkable differences in the rates were found between 7 kinds of pure metals, and the metals with higher boiling points had lower ablation rates, except for Cu. The LA/ICP-MS has been applied to depth analysis of TiN-coated steel sheet and painted steel sheet.View full abstractDownload PDF (1270K) -
Yumi MIYAMOTO, Tsuyoshi YAITA, Yuko SAITO, Kan KIMURA1991 Volume 40 Issue 12 Pages 883-888
Published: December 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe fission track method has been used for the determination of uranium in solid samples, but it has been hard to apply to the solution sample and to the solid sample in which uranium distributes heterogeneously. In the present study, we contrived the following sample preparation to give homogeneous distribution of uranium on the surface of a filter paper. GSJ rock samples (50100mg) were dissolved in a mixed acid of hydrofluoric acid, nitric acid, hydrochloric acid and perchloric acid. The solution was evaporated to dryness, and the residue was taken up with 1M nitric acid to prepare the samplesolution. An aliquot (100μl) of the sample solution was put on a filter paper (1.3×1.3cm) and dried up. This filter paper was contacted with a mica detector (5×5mm) that had been annealed for 6h at 600°C and etched by hydrofluoric acid for 23 h at 25°C in advance, and irradiated for 590 s at a neutron flux of 4.5×1013cm-2s-1. After irradiation, the mica detector was etched again. Double-etched latent tracks were more enlarged and therefore we could distinguish easily the latent tracks from the neutron induced ones. Track densities were determined using an optical microscope of 150600 magnification. Calibration curve was prepared with standard solutions. Then we determined uranium concentrations of GSJ rock samples and the values were in good agreement with reference values reported by Geological Survey of Japan.View full abstractDownload PDF (977K) -
Yutaka ASAHI, Masami TANAKA, Mayumi SUGIMOTO1991 Volume 40 Issue 12 Pages 889-893
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSulfa drugs were usually determined by alkaline titration or diazotization titration in Japanese Pharmacopoeia. Aim of this study was to confirm advantage of nonaqueous titration of sulfa drugs. Fourteen sulfa drugs were determined by potentiometric titration with perchloric acid in glacial acetic acid, acetonitrile and acetic anhydride. Sulfanilamides with very weak basic substituents such as sulfamethizole(I), sulfamethoxazole(II), sulfisoxazole(III), sulfacetamide(IV), sulfabenzamide(V), sulfathiazole(VI), sulfadiazine(VII) and sulfachloropyridazine(XIV) were titrated with 1eq. perchloric acid per 1mol bases in glacial acetic acid. Basic substituents such as pyrimidines and pyridazines in sulfamerazine(VIII), sulfamethazine(IX), sulfisomidine(X), sulfadimethoxine (XI), sulfamonomethoxine(XII) and sulfamethoxypyridazine(XIII) were titrated with 1eq. perchloric acid per 1mol bases in acetic anhydride immediately after the primary amino groups were acetylated. Standard deviation of this method was ca. 0.2%. It was estimated from the potential of glass electrode at the half equivalent point that the order of basic strength was sulfanilamide, dimethylpyrimidine(X, IX), methylpyrimidine(VIII), pyrimidine(VII) and chloropyridazine(XIV).View full abstractDownload PDF (765K) -
Hitoshi UEMORI, Kimiko YOSHIDA, Masami FUKUMOTO, Kunio TAKIUTI, Shuji ...1991 Volume 40 Issue 12 Pages 895-898
Published: December 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSWe have developed an improved method for the determination of organic solvent metabolites(HAs), hippuric acid(HA), mandelic acid(MA), ο-methylhippuric acid(ο-MHA), m-methylhippuric acid (m-MHA), p-methylhippuric acid(p-MHA) and creatinine(CR), in urine by reversed phase HPLC. The separation was carried out with a stainless-steel column (4.0mm×200mm) packed with Wakosil II-5C18-100 and 8% 2-propano1/10mM phosphate buffer (pH2.4) containing 6mM 1-octanesulfonic acid sodium salt as a mobile phase (1.0ml/min). A UV monitor (210 nm) was used for monitoring. Reproducibility of this method was excellent. Calibration plots between 10 and 1000ng/injection were linear and passed through the origin of the coordinate system. This method was used for the determination of HAs in urine on volunteers.View full abstractDownload PDF (502K) -
Yoshihito SUZUKI, Hitoshi KOIZUMI, Kazue TANI, Mingyu DING1991 Volume 40 Issue 12 Pages 899-905
Published: December 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSBoth suppressor system and non-suppressor system have been usually employed in ion chromatography. The latter system has used an organic acid solution as an eluent because of low conductance. The solvent strength and property of organic acids such as phthalic acid and heptafluorobutyric acid, change as the temperature changes. So it is necessary to investigate the effect of column temperature on anion chromatographic separation. In this study, the chromatographic separations of common inorganic anions and organic acids have been carried out on the two high performance hydrophilic anion exchange columns (Yokogawa SAM-3 and Tosoh TSKgel IC. Anion-PW) by using potassium biphthalate eluent at column temperature ranging between 10 and 60°C. The retention time of citric and tartaric acid increased with an increase in column temperature, and their behavior differed from those for the other organic acids tested. On the other hand, only sulfate in inorganic anions was specific in retention behavior, and its retention time increased with an increase in column temperature. But the other anions showed an opposite tendency. The effect of column temperature on thermodynamic parameters, resolution, height equivalent to a theoretical plate (HETP) and peak symmetry were discussed.View full abstractDownload PDF (1037K) -
Masako MIZUNO, Kenji TOCHIGI, Masahito ITO, Junkichi MIURA1991 Volume 40 Issue 12 Pages 907-912
Published: December 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSGlycated hemoglobins (GHb) in blood are composed of A1a, A1b, labile-A1c (l-A1c), stable-A1c (s-A1c) and others. It has been reported that the concentration of s-A1c is related to the average blood glucose value for the preceding 2 months, and the determination of s-A1c is useful for the assessment of long-term control of diabetes mellitus.Packing materials of various pore diameter, poly-methacrylate gel modified with carboxymethyl groups, were prepared. Particle diameter and ion exchange capacity of packing materials were 3.73.9μm and 0.260.29meq/g, respecttively. A correlation between pore diameter of packing materials and chromatographic performances, such as number of theoretical plate (N), retention time (tR) and pressure drop (ΔP) were studied. In result, it was apparentthat N was mainly dependent on pore diameter, and packing material of 800Å pore diameter gave best resolution. The column packed with packing materials of 6001000 Å pore diameter, showed N larger than 900 plates for s-A1c by linear gradient elution. Six hemoglobin components, A1a, A1b, HbF, 1-A1c, s-A1c and A0, could be separated in 3.5 min cycle by three step gradient elution.View full abstractDownload PDF (785K) -
Akira MACHINO, Hideo SUGIMOTO, Daijiro TERASAKI1991 Volume 40 Issue 12 Pages 913-916
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSTracer gases such as SF6 and CH4 have often been used to measure infiltration rates of indoor air. These gases have generally been measured by infrared spectroscopic analysis. Use of this method, however, sometimes causes problems because a lot of sample gases are required. On the other hand, a portable gas chromatograph has been developed in our previous work, that is equipped with a short-length capillary column and a micro thermal conductivity detector. This paper then refers to an application of the gas chromatograph to measure several sorts of tracer gases. Study was focused both on the optimum condition of tracer gas analysis and on their calibration method using air as a reference gas. It was consequently found that the introduction of PoraPLOT Q of 8 m length to the capillary column could shorten analysis time up to 1 min to analyze the tracer gases such as CH4, N2O, SF6 and C2H4. Thermal response values of the tracer gases against air (nitrogen+oxygen) under the optimum condition were obtained. The determined values of the tracer gases; using these values, agreed with those using a reference gas mixture. This result suggests that the calibration method by the use of thermal response values of the tracer gases is able to apply to the quantitative analysis of several sorts of tracer gases. It also appeared that the lower limits of detection of N2O and SF6 were enhanced to 2 ppm.View full abstractDownload PDF (530K) -
Shigeo TANUMA1991 Volume 40 Issue 12 Pages 917-920
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSQuantitative electron microprobe analyses of thin films of Mn-Bi and Co-Pt alloys on SiO2 substrates based on Gaussian ionization distribution models, were carried out. The used Gaussian models were the Wittry model and a normalized ionization distribution model proposed by the author. The resulting concentrations of Mn in Mn-Bi and Co in Co-Pt films and their thickness were compared with those by Rutherford backscattering (RBS) and Monte Carlo methods for electron microprobe analysis. The root mean square (RMS) differences of the analytical results of concentrations for thin films to the RBS results were 11.3% for the Wittry model and 4.6% for the normalized ionization distribution model. The RMS differences between the analytical results regarding the thickness of the thin films were 4.2% for the Wittry model and 7.9% for the normalized ionization distribution model. The RMS differences of the Monte Carlo method to the RBS method was 3.5% for the composition and 11.7% for the thickness. The resulting values for the composition by the normalized ionization distribution model were as good as those by Monte Carlo methods. In analyses of the thin film thickness, the Gaussian-type ionization model gave better results than the Monte Carlo method did. Therefore, the Gaussian-type normalized ionization distribution model can be applied to practical analyses of the composition and thickness of thin films on substrates.View full abstractDownload PDF (512K) -
Yasushi NAKAMURA, Shigenori MAEDA, Iwao NAGAI, Hisanari INOUE, Mitsuno ...1991 Volume 40 Issue 12 Pages T209-T215
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe precision and accuracy in the determination of impurities in copper and indium by glow discharge mass spectrometry (GDMS) were studied by the round robin test. Three copper wires (MBH Analytical Ltd., U.K.) and 1 indium wire (Nippon Mining Co., Ltd., Japan, 99.99%) used as samples for co-experiment were distributed to 5 laboratories.All analyses were carried out on the VG 9000 glow discharge mass spectrometers (VG Elemental, U.K.) using the so-called "MEGA Cell" (4 laboratories) and "SIMPLE Cell" (1 laboratory) as the glow discharge cell. The data of ion beam ratio obtained by using MEGA Cells showed no significant differences between 4 laboratories under different measurement conditions, and the relative standard deviations of interlaboratory were less than 17%. The relative sensitivity factors (RSF) for impurities in copper and indium were derived from these samples characterized by chemical analyses. There was a little difference between copper and indium matrix. Thus, the RSF should be determined from the analysis of standard reference materials comprised of the same matrix as samples in order to obtain accurate quantitative values by GDMS.View full abstractDownload PDF (936K) -
Hideo HARA, Fujiko SUZUKI, Rika SASAYAMA, Yoichi GOHSHI1991 Volume 40 Issue 12 Pages T217-T220
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA solid electrolyte sample is powdered by a vibrating mill in an agate pot. Then the powdered sample (0.2g) is decomposed with a mixed acid solution (20ml of hydrochloric acid +0.5ml of hydrofluoric acid and +1.0g of boric acid) in a Teflon bomb. After cooling, the solution was transferred into 250ml volumetric flask, and diluted to the mark with water, and analyzed by ICP-AES. The procedure described here provides a rapid and precise (RSD<2%) determination of lanthanum and strontium in the solid electro-lytes without erosion of glassware and quartzware (plasma torch, nebulizer etc.).View full abstractDownload PDF (516K) -
Takaho WATANABE, Masaharu TANAKA, Shu-ming CHEN, Chang-quig LIN, Yoshi ...1991 Volume 40 Issue 12 Pages T221-T226
Published: December 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSChlorine oxides were determined by amperometric titrator using current-integration method, and its experimental conditions were examined. Determination of chlorine oxides was based on iodometry. All of the hypochlorite and one fifth of the chlorine dioxide in the chlorine oxides solution could be determined at pH7, and the remaining chlorine dioxide and all of the chlorite could be done at pH2. Chlorine dioxide could be separated from chlorine oxides, such as hypochlorite, chlorite and chlorate, by aeration with nitrogen. The measurement of chlorine oxides was not influenced very much by ions, such as sodium, magnesium, potassium, calcium, zinc, lead and sulfur, and by glycine and glucose. In the presence of ferric, zinc and copper of 10ppm, chlorite could be determined using cation-exchange resin. Relative standard deviation for the determination of chlorine dioxide was 0.9%. Therefore, this highly sensitive method proved to be able to determine the chlorine oxides without pretreatment.View full abstractDownload PDF (1004K)
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