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Volume 43, Issue 3
Displaying 1-13 of 13 articles from this issue
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Takeshi ADACHI, Nobuo YUNOKI, Yuji ITO, Hidefumi HAYASHI1994 Volume 43 Issue 3 Pages 189-194
Published: March 05, 1994
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSProstaglandins (PGs; PGA1, PGB1, PGD2, PGE1, PGE2 and 6-keto-PGF1α) have been determined by LC/APCI-MS. The positive ion spectra obtained for PGs except for PGB1 exhibited base peaks corresponding to ions arising from the loss of H2O from the (M+H)+ and, when the solution containing AcONH4 as mobile phase was used, ions from the addition of NH4+. However, only PGB1 showed the protonated ion (M+H)+ as a base peak. The detection limits of each of the PGs were about 100 ng (on-column) by TIC (total ion current) mode and on SIM (selected ion monitoring) mode, good correlation factors were obtained for each of the PGs (γ>0.998). The detection limits and the relative standard deviations were 26 ng (on-column) and about 5% (n=5), respectively.View full abstractDownload PDF (765K) -
Nobuo UEHARA, Masayo HIROTA, Yoshio SHIJO1994 Volume 43 Issue 3 Pages 195-201
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSeveral hydrazones having similar structures and different donating atoms were synthesized and used as precolumn chelating agents of metal chelates for HPLC. The relationship between the HPLC selectivities for metal chelates and the donating atoms of hydrazones was also evaluated. The hydrazones were synthesized from corresponding hydrazines and aldehydes by refluxing in ethanol. Hydrazone chelates was insoluble in water. The chelates were prepared with methanol-water mixture or dimethylform-amide-water mixture. Most of the hydrazone chelates had absorption maxima near 400 nm. The eluents were methanol-water mixtures, which contained tetrabutylammonium bromide as necessary. The HPLC selectivities of hydrazones for metal ions were higher than the selectivities of complexation. The tridentate hydrazones gave more chelate peaks than the bidentate hydrazones did. The hydrazones made from 4-phenyl-3-thiosemicarbazide gave more peaks than the hydrazone made from benzoylhydrazine.View full abstractDownload PDF (1082K) -
Katsuo MURATA, Shinsuke YAMASHITA, Nobuaki OGAWA, Kazuichi HAYAKAWA, H ...1994 Volume 43 Issue 3 Pages 203-207
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSCopper plates were exposed to the ambient atmosphere in locations at different distances from the Sea of Japan coastline in order to investigate metal corrosion characteristic of weathering in winter. The samples from along the Sea of Japan coastline at Akita, Kanazawa, and Tottori districts were compared with those of Naruto district. The samples were analyzed by FT-IR reflection absorption spectroscopy (RAS). The formation of sulfato complexes and hydroxy species as well as oxides of Cu2O and CuO was observed on the samples in all regions, but the formation rate of their species was different. The formation rate of the species from samples along the Sea of Japan coastline rapidly proceeds while that of the samples in Naruto district proceeds slowly in the winter season. Polishing the surface of the copper plate with emery paper revealed that an oblique baseline observed in the IR-RAS spectrum of the corroded samples is attributable to roughness on the surface of the copper plates which is mainly caused by weathering.View full abstractDownload PDF (633K) -
Chiori YAKAWA, Hiroshi SANO, Hirokazu SASAKI, Toshiro NAKAYAMA1994 Volume 43 Issue 3 Pages 209-214
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSIMS was applied to quantitative depth profiling of yttria-stabilized zirconia film. We studied problems involved in the SIMS quantitative analysis of insulating materials, such as the electrical charge buildup on the surface induced by the bombarding ion beam and the matrix effect on the secondary ion yield. The electron flood proved to effectively neutralize the charge on the surface. The relationship between the secondary ion intensity and the yttria concentration was investigated using calibration standards prepared by sintering binary mixtures of yttria and zirconia. The resulting calibration curve showed that the relative secondary ion yield was not affected by the matrix composition over a wide concentration range and the yttria concentration could be determined by means of a linear equation. Increase of the ion yield in the presence of oxygen results in suppression of the matrix effect. The quantitative results obtained by SIMS were consistent with those obtained by EPMA and ICP-AES. SIMS is expected to be applied to the analysis of many kinds of materials.View full abstractDownload PDF (958K) -
Kunikazu IDE, Masataka KUDO, Takeshi KOBAYASHI, Shin-ichi HASEGAWA, Ha ...1994 Volume 43 Issue 3 Pages 215-221
Published: March 05, 1994
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSAn analytical method has been developed for the direct determination of trace amounts of zinc in sample solutions of nickel-based heat-resisting alloys without any preseparation. The samples contain complex alloying elements so it is necessary to use hydrofluoric acid for their decomposition. The interferences from such coexisting elements and hydrofluoric acid have been able to be overcome by the use of a L'vov platform and a peak area measurement. There were no adverse effects from diverse elements of 520% Co, Cr, Fe, Mo, W, Al, Mn, Nb, Ta, Ti and Zr. As for background correction an AC Zeeman effect method was found to be better than a continuum source method which showed an over correction. The established analytical procedure is as follows: 0.5 g of an alloy sample is decomposed with 4 ml nitric acid, 4 ml hydrofluoric acid and 5 ml distilled water by heating on a hot plate and the solution is then made up to 50 ml in a polypropylene volumetric flask. Ten microliters of the liquid is injected onto a L'vov platform in a graphite tube. The optimum operating conditions of AAS are ashing temperature, 650°C (20 s-20 s); atomizing temperature, 1350°C (0 s-5 s) and wavelength, 213.9 nm. Calibration solutions are prepared by adding a standard zinc solution to nickel matrix solutions. The sensitivity (absorbance, 0.0044) was 0.3 pg and the limit of detection was 0.8 pg (3σ of blank value) which was equivalent to 0.004 ppm in a sample. The proposed method is able to be applied to many kinds of nickel-based heat-resisting alloys.View full abstractDownload PDF (1078K) -
Yasuhisa SHIBATA, Naoto OKI, Satoshi OZAWA, Hiroyuki MIYAGI1994 Volume 43 Issue 3 Pages 223-229
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA study into how selectivity affects the accuracy and precision of chloride ion-selective electrodes (Cl-ISEs) used in the analysis of physiological fluids is presented. In this study, dimethyldioctadecyl-, tetraoctadecyl- and methyltridodecylammonium salts (DMDODA, TODA and MTDDA, respectively) were used as sensing materials. Control serum and healthy human urine samples were analyzed by Cl-ISEs and the interfering anions in these samples were examined by ion chromatography in order to study the relation between error and selectivity. It was found that errors in the analysis of these samples were mainly due to the sulfate ion, because good correlation between its concentration and error was observed. From the comparison of selectivity and Syx (standard deviation of y on x) obtained by three types of sensing materials, it was shown that a highly reliable Cl-ISE could be produced by an improvement of selectivity to hydrophilic anions such as sulfate ion without a strong affinity for lipophilic anions. Furthermore, it was also suggested that Cl-ISE should have a small selectivity factor to organic acid anions and drugs. The Cl-ISE based on TODA exhibited excellent selectivity and was applied to the analysis of patient physiological fluids (serum, plasma, urine); good accuracy and precision were obtained. Therefore, it is expected to be useful in the field of clinical analysis.View full abstractDownload PDF (1053K) -
Noriko OHNO, Hiroatsu SAKAI, Hiroshi OHTA, Tadao SAKAI1994 Volume 43 Issue 3 Pages 231-235
Published: March 05, 1994
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA rapid and sensitive determination of acrinol in pharmaceuticals was investigated by spectrofluorometric flow injection analysis. The single flow system was assembled to depress dispersion of the sample solution. The sample was dissolved in the buffer solution (pH 4) and acetone to give 30 v/v% acetone solution and 100 μl of sample solution was injected into the buffer stream. The mixing coil was 1 m in length. The fluorescence intensity of acrinol was measured at excitation and emission wavelengths, 366 and 496 nm. The intensity was enhanced by adding polar solvents such as methanol, ethanol, 1-propanol and acetone. Of these solvents, the 30 v/v% acetone solution was most effective. The calibration graph showed a good linear relationship between 1×10-9 M7×10-8M of acrinol and the dynamic range was wide. The sensitivity was enhanced about 1000 times by the colorimetry compared with other methods. The lower detection limit was 7.5×10-10M (S/N=3). The relative standard deviation was 0.5% for 10 repeated runs of 5×10-8 M acrinol and a sampling rate of 60/h. Many substances such as berberine and dibucaine showed fluorescence, but had different excitation and emission wavelengths. Accordingly, these substances did not interfere with the determination of acrinol. The proposed method can be successfully applied to the rapid, accurate and trace determination of acrinol in pharmaceuticals with a diversified matrix.View full abstractDownload PDF (736K) -
Kazuyoshi FUJIMURA, Noriyuki WATANABE, Tsuguo SAWADA1994 Volume 43 Issue 3 Pages 237-240
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA study to find a better mobile phase for use in the rapid determination of inorganic anions such as fluoride, chloride, nitrite, phosphate, nitrate and sulfate ions by indirect photometric ion chromatography is presented. The eluent optimized was a weak-alkaline (pH 7.3) buffer solution containing 0.7 mM potassium hydrogenphthalate-0.1 mM sodium tetraborate-0.5 mM boric acid-0.1 mM HEPPS-0.05 mM sodium hydrogencarbonate-5 % butanol. The problem of the system peak otherwise encountered was eliminated by judicious choice of the alkalinity of the buffer solution. The eluent did not show any pH drift typically caused by dissolution of carbon dioxide, and was able to separate the phosphate ion completely from the chloride. Whole anions above described were determined within 15 min.View full abstractDownload PDF (425K) -
Noriko NAKAYAMA, Osamu MACHINAGA, Yoshio AOYAMA1994 Volume 43 Issue 3 Pages 241-246
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn application of the alizarine complexone (ALC) photometric method using a succinic acid-hexamethylenetetramine buffer (pH 4.6) and ion chromatography (IC) for the determination of fluoride in gypsum has been studied. A sample was decomposed with HCl. For the spectrophotometry, acethylacetone was added to a portion of the neutralized solution and its absorbance was measured using La-ALC photometry. For IC, after dilution and pretreatment on a column packed with cation-exchange resin of the silver form, the sample solution was injected into the system. The analytical results agreed well with the values by the JIS method. These methods are rapid and useful.View full abstractDownload PDF (960K) -
Sanae IKEDA, Hiromu SATAKE1994 Volume 43 Issue 3 Pages 247-250
Published: March 05, 1994
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSAn apparatus for the flow injection analysis of L-cystine using an amperometric detector composed of a glassy carbon electrode and a silver wire electrode was constructed, and the optimum conditions were investigated. The carrier solution used was a mixture of 0.6 M H3BO3, 0.1 M Na2B4O7·10H2O and 0.15 M Na2SO3, at a flow rate of 3.0 ml/min. A hundred microliters of L-cystine solution (10-410-3 M) was injected into the flow system at an applied potential of 0.55 V, and the indicator current was recorded after the reaction with sulfite in the reaction coil (150 cm). L-Cystine (0.3600.841 μg) was determined with a relative error of 0.5% and RSD of 0.7%. This apparatus made it possible to determine 30 samples in one hour.View full abstractDownload PDF (544K) -
Toshikazu TABATA, Kimihiko TAKADA, Yoshiaki ITO, Yukio SHOJI, Kei SAIT ...1994 Volume 43 Issue 3 Pages 251-254
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSVitamin A contents are often determined by high performance liquid chromatography in laboratories, but a reference standard is available only for thin layer chromatography. A vitamin A acetate reference standard was prepared by diluting retinyl acetate to 200000 IU/g with medium chain triglyceride (MCT) and was packed in a gelatin soft capsule. This reference standard was evaluated in 10 laboratories by UV and HPLC methods. Stability testing was carried out with this sample stored at 5°C, 25°C and 40°C for 24 months. It was proved that this standard is useful if stored at 5°C for at least 2 years.View full abstractDownload PDF (464K) -
Naoki HIRAYAMA, Minemasa HIDA1994 Volume 43 Issue 3 Pages 255-258
Published: March 05, 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (631K) -
1994 Volume 43 Issue 3 Pages e1
Published: 1994
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (106K)
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