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Volume 39, Issue 8
Displaying 1-12 of 12 articles from this issue
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Toshiyuki MITSUI, Munemasa HIDA, Yoshikazu FUJIMURA1990 Volume 39 Issue 8 Pages 427-431
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSMultivariate analysis was applied to identification of fibers using a personal computer. Individual pyrograms of 37 known fibers were obtained by pyrolysis GC. These pyrograms were divided into twelve sections in terms of retention time in each pyrogram. In all pyrograms, relative values (16) were given for each of 24 sections based on the peak height or peak area. These data were used for the multivariate analysis such as cluster analysis, quantification IV, principal component analysis and factor analysis. Unknown samples were compared with the 37 known fiber samples, using cluster distance, principal component score and factor score.View full abstractDownload PDF (707K) -
Tomoo MIWA, Xingen YU, Mitsuaki MURAKAMI1990 Volume 39 Issue 8 Pages 433-437
Published: August 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSCopper cations and readily dissociable copper complexes at the fractional ppb level in river water have been directly determined in the presence of humic substances by differential pulse anodic stripping voltammetry (DPASV) with Nafion (perfluorosulfonic acid polymers) coated mercury film glassy carbon fiber electrodes (NCMF-GCFE, GC-20, ca. 10μm diam.×1 mm). An aliquat of water sample (100 ml) is filtered through a 1-μm Nuclepore polycarbonate membrane filter to remove suspended particulate matters, and the filtrate is prepared to 0.01 M KNO3-0.001 M KCl solution (pH 5). Copper in the electrolyte is electrodeposited on the NCMF-GCFE at -1.0 V vs. Ag/AgCl for 10 min passing through the flow electrolysis cell at a flow rate of 3.3 ml min-1. The electrode potential is then scanned to zero volt at a rate of 50 mV s-1, a differential pulse anodic stripping voltammogram being recorded. The electrode is held at this potential for 10 s to use the next deposition/stripping cycle. The analytical results for the river water obtained by the proposed method are in fairly good agreement with those obtained by DPASV using a hanging mercury drop electrode in 0.01 M KNO3 (pH 5) after removal of humic substances with an anion exchanger (DEAE-Sephadex A-25).View full abstractDownload PDF (787K) -
Kaneharu KATO1990 Volume 39 Issue 8 Pages 439-444
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn analytical method combined chlorination separation of matrix with ICP-AES has been developed for reactor grade Zr alloys (Zircaloy-2). A sample (1 g) is taken into a Pt boat and chlorinated with HCl gas of 100 ml/min in a glass reaction tube at ca. 330°C. Matrix Zr of the sample is volatilized and separated as ZrCl4. The analyte elements remaining quantitatively as chlorination residue are dissolved in a mixture of mineral acids (6 M HCl 3 ml + conc. HNO3 0.5 ml + conc. H2SO4 0.2 ml) and diluted to 20 ml with distilled water after filtration. ICP-AES was used for simultaneous multielement determination using a calibration curve method. The present method has the following advantages: simple sample preparation procedure; applicability to any form of samples to determine multielements; simple ICP-AES calibration procedure. This method was successfully applied to the determination of Fe, Ni, Cu, Co, Mn and Pb in the Zr alloys of JAERI CRM's and NBS SRM's.View full abstractDownload PDF (833K) -
Yoshiko BABA1990 Volume 39 Issue 8 Pages 445-449
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe determination of phosphorus in tissues by the flushed oxygen combustion method was investigated. Phosphorus oxides produced by the combustion of the samples were washed out from the combustion tube and the boat. The solution containing metaphosphoric acid was then heated on a water bath for hydrolysis. After cooling, phosphate was determined spectrophotometrically as phosphovanadomolybdate. Most phosphorus oxides produced by the combustion of triphenylphosphine adhered to the wall of the combustion tube. Adenosine triphosphate disodium salt remained as phosphorus oxides in the boat. Most phosphorus oxides formed by the combustion of a liver sample remained in the boat. The combustion behavior of phosphorus oxides proved to be the characteristic of the substance.View full abstractDownload PDF (645K) -
Takao KATASE, Eitaro WADA1990 Volume 39 Issue 8 Pages 451-456
Published: August 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSWe studied on an isolation of chlorophyll a for determination of stable isotope ratios of carbon (δ13C) and nitrogen (δ15N) and applied it to determine in Microcystis spp. from Suwa lake, Japan. The algae were collected four times between June and September, 1987 by using a 20l plankton net (40μm, mesh size). Collected freezed-samples (7.320.6 g, wet base) ground with anhydrous Na2SO4 using a mortor and a pestle were extracted with acetone (200 ml). The extracts were precipitated with 1, 4-dioxane (crude chlorophyll) and consequently purified chlorophyll a (2.38.1 mg) was obtained quantitatively by successive chromatography with DEAE-Toyopearl 650 M (2288μm) and Sepharose CL6B (45165μm) packed in glass tubings. The ratio, (δ13C, ‰ ) of chlorophyll a in the algae had changed from -33.8±0.05 in June 19 to -27.5±0.3 September with different growth. Difference (Δ13C) between δ13C of chlorophyll a and that of a whole body of the algae had also changed from -9.4±0.05 to -3.4±0.1.Comparing to the carbon ratios, the both ratios of δ15N and Δ15N slightly changed from 22.0 to 23.5 and 12.9 to 16.0, respectively. The change of heavy isotopes in Δ13C and Δ15N was reverse: The heavy carbon was depleted and heavy nitrogen was enriched.View full abstractDownload PDF (986K) -
Kazutoku OHTA, Haruo MATSUI, Kazuhiko TANAKA1990 Volume 39 Issue 8 Pages 457-461
Published: August 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA new type electodialytic membrane suppressor (EDMS) based on electrodialysis with cation-exchange membrane at constant applied potential has been developed for anion chromatography with conductometric detection. The EDMS consists of an anode, a cathode, a cation-exchange membrane in the H+-form, and a sulfuric acid regenerant flow passage. When carbonate/hydrogen carbonate eluent and sample anions were introduced into the EDMS, the eluent and sample anions were converted to carbonic acid and the corresponding acids, respectively, by the H+ ion of the regenerant through the cation-exchange membrane. When 1.6 mM Na2CO3/2.0 mM NaHCO3 eluent was used for the anion chromatography using the EDMS, the eluent conductivity decreased from about 570 to 13μS/cm, with enhancement of conductivity for the anions, at applied potential of approximately 5 V. The use of EDMS showed much smaller eluent conductivity in comparison with that (42μS/cm) by the conventional cation-exchange membrane suppressor. The EDMS was successfully applied to the anion chromatographic determination of several anions in rain and soil waters.View full abstractDownload PDF (849K) -
Masakazu DEGUCHI, Tomomi KITABAYASHI, Kiyotoshi MORISHIGE, Kenji YAMAG ...1990 Volume 39 Issue 8 Pages 463-466
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIndium reacts quantitatively with 2-hydroxy-5-sulfoaniline-N-salicylidene (HSS) to form a fluorescent complex at pH 5.05.2. In 8 v/v% N, N-dimethyl-formamide (DMF), the fluorescence intensity of the complex is stable for at least 72 h. The analytical procedure is as follows: To a sample solution containing less than 10μg of indium, were added 1 ml of 0.1 w/v% sodium fluoride solution, 2 ml of 0.1 w/v% HSS solution in DMF and 1 ml of 0.2 w/v% ammonium acetate solution. The pH of the solution was adjusted to 5.1±0.1 with ammonium hydroxide or hydrochloric acid and then the solution was diluted to 25 ml with water. After standing for 15 min, the fluorescence intensity was measured at 500 nm with excitation at 405 nm. By the use of 0.01, 0.05 or 0.1μg/ml uranine solution as a setting reagent, 0.0310μg of indium was determined. The relative standard deviation was 0.6% (n=5) for 1.6μg of indium. Aluminium (III), gallium (III) and tin(II) gave serious positive errors. The proposed method was successfully applied to the determination of indium in zinc residue, where the indium was previously separatedfrom interfering elements by extraction with isopropylether.View full abstractDownload PDF (456K) -
Seiji YASUDA1990 Volume 39 Issue 8 Pages 467-469
Published: August 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe chemical shifts and profile changes in the chlorine Kα and Kβ X-ray emission spectra from solid organic chlorine compounds were measured with a two-crystal X-ray spectrometer. The chlorine Kα1 peaks shifted successively to higher energies with increasing electronegativity of the atom bonding to the chlorine from H to S, C and N atom. Similar tendency was found in the chemical shifts of the chlorine Kα4 satellite and Kβ1 peaks. Most of the organic chlorine compounds studied here exhibited the chlorine Kβ1 peak in the higher energy region than that of sodium chloride. The Kβ profiles of chlorine in organic compounds revealed much more complicated structures with the high and low energy satellites. The high energy satellite Kβx was observed for chlorine bonded directly to benzene ring and N atom. These spectral changes might be used to estimate the chemical bonding states of chlorine in a variety of solid organic samples.View full abstractDownload PDF (426K) -
Eiko NAKAMURA, Hiroshi NAMIKI1990 Volume 39 Issue 8 Pages 471-473
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSTo determine trace silicate in highly purified water, conditions for the extraction of Heteropoly Blue into 1-butanol were investigated. A sulfuric acid concentration of 1.3 M was proposed for the extraction. The recommended procedure is as follows. Two hundred milliliters of a sample solution is taken in a 300 ml Teflon separating funnel and 4 ml of an ammonium molybdate (20%) -H2SO4 (2.5 M) solution is added. The solution is left standing for 20 min to form molybdosilicic acid completely. After the addition of 25 ml of H2SO4 (2+1) and 2 ml of L-ascorbic acid solution (10%), it is left standing for 10 min to develop Heteropoly Blue. Twenty five milliliters of 1-butanol is added to the solution which is shaken for 2 min. The absorbance of the Heteropoly Blue extracted into the organic layer is measured at 800 nm. For the reagent blank test, 4 ml and 8 ml of the ammonium molybdate-H2SO4 solution are added respectively to two 200 ml portions of water. The absorbances, A1 and A2, for the two solutions are measured as mentioned above. The difference, A2-A1, corresponds to the absorbance due to 4 ml of the ammonium molybdate-H2SO4 solution. The absorbance obtained on a sample is corrected by subtracting the A2-A1 value. Silicate in some highly purified waters was determined to be over the range of 225μg of SiO2/l.View full abstractDownload PDF (336K) -
Yukikazu HATTORI, Hitoshi YAMAMOTO, Kanji NAGAI, Kiyoko HAGINO, Masao ...1990 Volume 39 Issue 8 Pages T113-T116
Published: August 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSLow molecular weight halogenated hydrocarbons (LMHs) in industrial water and waste water have been determined according to JIS K 0125, in which a packed column has been used as the GC column. In this report, wide bore capillary columns were evaluated as a GC column. DB-624 showed the best separation ability of 5 kinds of column (DB-1, DB-5, DB-17, DB-624, DB-WAX). When hexane solution of LMHs was measured with DB-624, the relative standard deviations (RSD) of response (peak height) and retention time (RT) were 0.82.1% and 0.51.4%, respectively. When the head space method was used, the RSDs of response and RT were 3.45.0% and 0.040.20%, respectively.View full abstractDownload PDF (540K) -
Yukinori MATSUZAKI, Kazuhiro YANAGISAWA, Yasushi NAKAMURA1990 Volume 39 Issue 8 Pages T117-T120
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA method for the determination of zeatin (Z) and 6-benzylaminopurine (BA) in culture medium solutions containing a high concentration of saccharides and salts was studied. A medium sample solution containing of Z or BA was passed through an octadecylsilyl-bonded silica cartridge column. The analytes were then eluted from the cartridge with 50% acetonitrile. The eluate was dried up by a rotary evaporator. After the residue was dissolved in 10% methanol, Z or BA was determined by HPLC. The determination limits in the medium were 0.6 ng/ml and 0.9 ng/ml for Z and BA, respectively.View full abstractDownload PDF (490K) -
Kazuo IMAEDA, Takaho WATANABE, Masaharu TANAKA, Yoshihiro YOSHIMURA, K ...1990 Volume 39 Issue 8 Pages T121-T124
Published: August 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSChlorine dioxide, which inactivates bacteria and viruses over a broad pH range and does not produce trihalomethanes, can be used for disinfection of drinking water. Commercially available instruments based on amperometric titration lack sensitivity for the determination of chlorine oxides. We developed an amperometric titrator (AT) using a current-integration method in order to increase sensitivity for the determination of oxidized chlorine species. The AT consists of capacitors, an electrometer, a D/A converter, logic control circuit, a track/hold and a digital voltmeter. A constant voltage generated by the D/A converter is applied between a pair of platinum electrodes. The capacitor integrates diffusion current. The electrometer measures the terminal voltages of the capacitors. Minimum resolution for AT was a few pA. The relative standard deviation of the titration was less than 0.2%. Detection limit of iodine measurement was 5 ppb.View full abstractDownload PDF (584K)
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