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Volume 39, Issue 1
Displaying 1-15 of 15 articles from this issue
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Hiroyasu ITO, Akio YASUHARA, Masatoshi MORITA, Tsuguo MIZOGUCHI, Kinji ...1990 Volume 39 Issue 1 Pages 1-5
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSRelative intensity of three dominant ions per mole in mass spectra of many halogenated benzene compounds, compared with ion at m/z 172 in the mass spectrum of 2-fluorobiphenyl (internal standard), has been measured by using mass chromatography in capillary GC/MS. Large variation of the relative intensity was obtained, but calibration curve showed linearity between 1100 ng of individual compounds. Relative intensity depended also upon molecular structure and/or chemical properties of the cpmpounds. Substitution by iodine atom in benzene ring enhanced the molar relative intensity of halogenated benzene compounds.View full abstractDownload PDF (675K) -
Masatomi SAKAMOTO, Yukio KOURA, Kenji HATANAKA, Tomitaro ISHIMORI1990 Volume 39 Issue 1 Pages 7-11
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA thermogravimetry for simultaneous determination of K, Rb and Cs has been studied with their tetraphenylborates (M[TPB]) and tetra(p-fluorophenyl)borates (M[F4TPB]). These three metal ions were completely recovered from a solution as M[TPB], whereas only Cs quantitatively as M[F4TPB] which contained a small amount of Rb[F4TPB]. About 10 mg of each precipitate was heated at a rate of 5.6°C min-1 in an air stream of 50 cm3 min-1. The amounts of K, Rb and Cs were determined by the equations. Experimental error was within 10% when the amount of each metal in 50 cm3 of sample solution was more than 5 mg.View full abstractDownload PDF (704K) -
Shigeru TANAKA, Kensuke YASUE, Yoshikazu HASHIMOTO1990 Volume 39 Issue 1 Pages 13-18
Published: January 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe four methods for the determination of formic, acetic, propionic, isobutyric and butyric acids in rain water by ion exclusion chromatography were investigated. In method (A) and (C), 0.05 mM H2SO4 was the eluent, and in method (B) and (D), 0.1 mM 1-octanesulfonic acid and 0.1 mM HCl were the respective eluents. Method (A) used Na2SO4 as the scavenger while the other methods used tetrabutylammonium hydroxide as the scavenger. Carboxylic acids were detected by conductivity detector (CD) and ultra violet detector (UV) at 210 nm. The analytical sensitivity of method (A) was the highest of the four methods in the case of detection by CD. However, the analytical sensitivities of the four methods by UV differed little. It is considered that the decrease in the analytical sensitivity of methods (B), (C) and (D) using CD was caused by ion association between tetrabutylammonium ion and carboxylic acid ion. The detection limits by CD were 0.0010.002 μg/ml for formic acid, 0.001 μg/ml for acetic acid, 0.0030.004 μg/ml for propionic acid, 0.0060.008 μg/ml for isobutyric acid and 0.0060.007 μg/ml for butyric acid. The detection limits by UV were inferior to those by CD. Repeatability of the analysis data for carboxylic acids in standard solutions was good. The concentrations of these carboxylic acids in 14 rain samples obtained at Hiyoshi, Yokohama, were measured from June to November, 1988 by using method (A). The concentration range was 0.071.98 μg/ml for formic acid. 0.030.85 μg/ml for acetic acid, 0.020.15 μg/ml for propionic acid, 0.060.44 μg/ml for isobutyric acid and 0.060.16 μg/ml for 1-butyric acid.View full abstractDownload PDF (896K) -
Hitoshi YAMAGUCHI, Takeshi KOBAYASHI, Kei YAMADA, Haruno OKOCHI1990 Volume 39 Issue 1 Pages 19-24
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe molybdenum disilicide is a material for very large-scale integrated circuits, and the determination of trace impurities in it is required. Graphite furnace AAS using a platform technique and ICP-AES have been investigated. The matrix element, molybdnum, was removed by cation exchange chromatography. Recoveries of over ca. 96% were obtained for Al, Be, Bi, Ca, Cd, Co, Cu, Fe, In, K, Mg, Mn, Na, Ni, Tl and Zn using a 0.05 M H2SO4 sample solution, while in the case of Ga, Ti and Sn, it was necessary to adjust the sample solution to 0.1 M H2SO4. The analytical range of contents was from 0.0 n ppm to 0.0 n %. The analytical procedure was as follows; 1.00 g of a sample was dissolved with HF-HNO3, 1.1 ml of H2SO4 (1+1) was added and the solution was heated until fuming appeared. After cooling, it was diluted to 200 ml (0.05 M in H2SO4). The solution was passed through a cation exchange column (Dowex 50-X4, 100200 mesh, 9 mm i.d., 13 ml) and the column was washed with 100 ml of 0.01 M HNO3-0.15% H2O2. The analytes were eluted with 90 ml of 2 M HNO3. The eluate was diluted to 100 ml and a 20 μl aliquot was injected into a graphite furnace. Residual solution was used for measurement by ICP-AES.View full abstractDownload PDF (888K) -
Chushiro YONEZAWA, Michio HOSHI1990 Volume 39 Issue 1 Pages 25-31
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSBlank values from quartz tubes used as sample containers for long-time irradiation in INAA were evaluated to study their effects on the analytical results. The main source of blank values, impurity contents and degrees of contamination before and during irradiation, were examined by INAA. The sample tubes and standards were irradiated in JRR-2 at a thermal neutron flux higher than 2×1013 n cm-2 s-1 for 265.5 h. After cooling for more than 20 d, the samples were etched up to a subsurface depth of 5 μm with 46% of hydrofluoric acid at room temperature. Then, the gamma-ray spectra were measured with a Ge(Li) detector. From the measurement of impurity distribution, the surface etching up to 5 μm with hydrofluoric acid was found to effectively minimize the blank values. Synthesized quartz tube (VIOSIL-F) from tetrachlorosilane was found to be the most suitable for INAA, as a result of impurity analysis of several kinds of quartz tube. Contamination by fission products from the U contained at ppb levels in Al capsules and wrapping foil was found with the long-time irradiation. Such contamination could be prevented by wrapping the quartz tube with polyimide film (75125 μm). Contamination from the blowing step during production of the ampoules from the quartz tube was also prevented by using a quartz gas burner. In INAA of 0.1 g of Bovine Liver (NBS SRM 1577) and Orchard Leaves (NBS SRM 1571), the blank values from the ampoule (VIOSIL-F 1.5 g) were minimized by the above procedure to less than 1% for all the elements determined except Cr.View full abstractDownload PDF (1085K) -
Yushi SHICHI, Yasuhide INOUE, Masaharu ARITA, Jyoji KUNIYA, Tadashi AS ...1990 Volume 39 Issue 1 Pages 33-36
Published: January 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe aim of this study is to analyze the degradation of Nylon 66 by means of the X-ray photoelectron spectroscopy (XPS) and other analytical methods. The sample was Nylon 66 without any additive which was degraded at 80, 100, 120 and 150°C. Quantitative analysis was carried out for elements arid atomic group on and inside the samples by XPS. Signals of the atomic groups were separated using peak fitting of Cls. The degrees of crystallization were analyzed by XRD and DSC. On the basis of the data obtained by this method, it was assumed that the heat degradation of the Nylon 66 surface was caused by simultaneous crystallization and oxidation reactions which produced carbonyl and carboxyl groups. The formation of carboxyl groups was confirmed at degradation temperatures higher than 120°C.View full abstractDownload PDF (548K) -
Kiyomi HAMAGUCHI, Toshihiko HANAI, Hiroaki KUBO, Toshio KINOSHITA1990 Volume 39 Issue 1 Pages 37-41
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSOptimal conditions of separation for isoniazid and acylisoniazid derivatives (acetylisoniazid, propionylisoniazid, isobutyrylisoniazid, butyrylisoniazid, benzoylisoniazid) were determined in reversed-phase ion-pair LC. Sodium dodecanesulfonate was the best ion-pair reagent among alkylsulfonates. When the carbon number of alkylsulfonate was below 4, the elution order was isoniazid, acetylisoniazid and propionylisoniazid. When the carbon number of alkylsulfonate was 5, the elution order of isoniazid and acetylisoniazid was changed. Further when its number was 8, the elution order of isoniazid and propionylisoniazid was reversed. The acyl group of acylisoniazid also affected their retention. The conditions of HPLC were as follows : Column, Inertsil ODS-2 (5 μm, 150×4.6 mm i.d.); eluent, 24% aqueous acetonitrile solution containing 2.0 mM sodium dodecanesulfonate (pH 3); flow rate, 1.0 ml/min; column temperature, ambient. Retention time was 6.30 min for isoniazid, 3.69 min for acetylisoniazid, 4.49 min for propionylisoniazid, 6.06 min for isobutyrylisoniazid, 6.25 min for butyrylisoniazid and 12.58 min for benzoylisoniazid. The capacity ratios (log k') of isoniazid and acylisoniazid derivatives and the partition coefficients measured in 1-octanol/water (log P') were in good linear relation with those calculated by Rekker's hydrophobic fragmental constants (log P). Coefficient of correlation for firstorder regression lines of log P-log P', log k'-log P and log k'-log P' plots were 0.984, 0.997 and 0.996 (n=6), respectively. This calculation method could generally be used to find an appropriate internal standard compound for reversed-phase LC.View full abstractDownload PDF (626K) -
Akinori ISOZAKI, Hajime SASAKI, Asako FURUKAWA, Satori UTSUMI1990 Volume 39 Issue 1 Pages 43-47
Published: January 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA simple method is investigated for direct determination of copper in silicate rocks by graphite furnace AAS. The method is based on the atomization of copper by the introduction of powdered rock samples suspended in 10% glycerin solution into a furnace. The sample (less than 10 μm in particle diameter) of 110 mg containing less than 1.0 μg of copper is placed in a polystyrene test tube fitted with a stopper (15 ml). 5.0 ml of 10% glycerin solution are added to the tube, and the sample is dispersed into solution by an ultrasonic agitator for 1 min. Then, 10 μl of the suspension, which has been mixed thoroughly to make a uniform suspension, are injected into a graphite furnace. The sample is initially dried at 400°C for 15 s, subsequently heated at 1200°C for 30 s, and copper is atomized at 2600°C for 10 s in an argon atmosphere (argon flow rate: 31/min). Peak areas of the copper signal at 324.7 nm are measured under background correction with the neon line at 320.8 nm. The relative standard deviation is 2.7% on 7 repeated measurements for the determination of 56 ppm copper in a standard silicate rock sample (JB-1).View full abstractDownload PDF (879K) -
Yoshifumi HARADA, Natsuko KURATA, Giichi FURUNO1990 Volume 39 Issue 1 Pages 49-54
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSImpurities (Al, Ba, Ca, Cr, Fe, Mg, Mn, Ni, Sr, Ti and Zn) in silicon nitride powder were determined by the following procedure: Fuse silicon nitride (0.5 g) with a mixture of sodium nitrate (1.5 g) and sodium carbonate (1.5 g) in a platinum crucible by raising the temperature to 1000°C. Dissolve the melt in water and make the solution acidic with hydrochloric acid. Then, add ethanol and boil it to reduce chromium(VI) to (III). After adding lanthanum ion (10 mg) and phenolphthalein indicator, make the solution alkaline by adding 2.5 M sodium hydroxide solution, an additional 4 ml being added after the solution changes to red, to redissolve the precipitate of silicic acid. Separate the precipitate of lanthanum hydroxide by filtration. Dissolve the precipitate into a small amount of hydrochloric acid, make the solution to 25 ml with water and determine the elements in the solution by ICP-AES. An oxidizing agent such as sodium nitrate should be employed in the fusion of silicon nitride; otherwise, the iron, copper, etc. in the silicon nitride would alloy with the platinum crucible. The recoveries of the elements from matrix components by the proposed method were 95100% in most cases, about 90% for aluminum and about 80% for chromium. This method was applied to the rapid determination of impurities in high-purity silicon nitride samples (99.9099.99%), and the results were in good agreement with those by the JIS method.View full abstractDownload PDF (874K) -
Shogo SUZUKI, Natsuko KATSURAGI, Shoji HIRAI1990 Volume 39 Issue 1 Pages 55-62
Published: January 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSMultielements in rock reference samples, JLk-1 (Lake sediment), JLs-1 (Lime stone), JDo-1 (Dolomite) and JP-1 (Peridotite) prepared by the Geological Survey of Japan (GSJ) were determined by instrumental neutron activation analysis (INAA). The GSJ rock reference samples (ca. 6688 mg) were irradiated for either a short time (30 s) or a long time (5 h) at Musashi Institute of Technology Research Reactor (MITRR). The samples were irradiated by two methods ; thermal neutron irradiation without cadmium filter and epithermal neutron irradiation with cadmium filter. The activated samples were measured by three methods; conventinal γ-ray spectrometry using a coaxial Ge detector, anticoincidence counting spectrometry and coincidence counting spectrometry using a coaxial Ge detector and a well type NaI(Tl) detector. γ-Ray spectra obtained were analyzed by a peak-fitting procedure using a GAMA system. Concentrations of 44 elements in JLk-1, 32 elements in JLs-1, 35 elements in JDo-1 and 24 elements in JP-1 were determined by the combination of these irradiation and counting methods with correction for deadtime and interfering nuclear reactions.View full abstractDownload PDF (1047K) -
Fractional determination of metallic copper, cuprous oxide and cupric oxide in copper oxide catalystYoshikazu KIKUTA, Hiromu SAKAMOTO1990 Volume 39 Issue 1 Pages T1-T4
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSMetallic copper, cuprous oxide and cupric oxide in a copper oxide catalyst were determined by combination of wet chemical method and XRD. The ratio of the copper metal to the copper oxide was obtained after treatment of the sample with HCl, where the oxides were dissolved with HCl. The ratio of the cuprous oxide to the cupric oxides was obtained by XRD. The ratio of the three components calculated with the above ratios well agreed with the results obtained by the reaction of this catalyst with hydrogen gas.View full abstractDownload PDF (490K) -
Motonori ETOH1990 Volume 39 Issue 1 Pages T5-T9
Published: January 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA sample was decomposed with aqua regia in a Teflon sealed vessel at 180°C for 5 h. Interferences by coexisting elements were significant in electrothermal AAS. Therefore, coprecipitation method with tellurium was used for separation of Au, Pt, Pd and Rh from the matrices. Small amounts of coexisting elements coprecipitated with tellurium were further eliminated by cation exchange separation. Silver was separated only by the cation exchange separation because of the poor recovery by tellurium coprecipitation. This method was applied to the Canadian certified reference materials, PTC and PTM, and analytical results were in good agreement with the certified values (R.S.D.: 35%).View full abstractDownload PDF (792K) -
Hiromu SATAKE, Sanae IKEDA1990 Volume 39 Issue 1 Pages T11-T16
Published: January 05, 1990
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSCoated-wire membrane electrodes for thiocyanate ion were developed by using commercial epoxy resin adhesive (rapid-cure type) as the sensing material membrane. The electrode structure is as follows. Electrode(1): silver/epoxy resin adhesive (epoxy resin: curing agent=1:1) membrane. Electrode(2): silver/silver iodide-polyvinylchloride type adhesive (AgI:90%) membrane/epoxy resin adhesive membrane. Electrode(3): silver/silver iodide (containing 0.5% potassium iodide)-polyvinylchloride adhesive membrane/epoxy resin adhesive membrane. It was found that the three electrodes showed the Nernstian response to thiocyanate at ion concentrations from 10-4 M to 10-1 M in 10-1 M disodium hydrogenphosphate. The variation of pH has no effect on the electrode potential over the range of pH 4 to 10 at thiocyanate ion concentrations from 10-3 M to 10-1 M. The order of the selectivity coefficients (Kij) for electrode (2) is as follows: Cl-_??_ClO4->I->NO3-_??_S2-_??_Br-_??_CN-_??_ClO3->CH3COO-_??_CO32-_??_BF4-_??_Fe(CN)64-_??_S2O32-_??_CrO42-_??_C2O42-_??_SO42-Selectivity coefficients of the three electrodes for the anions investigated were less than 0.5.View full abstractDownload PDF (901K) -
Yasushi NAKAMURA, Takayuki FUKUDA1990 Volume 39 Issue 1 Pages T17-T21
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe determination of trace amounts of As, Sb, Bi, Sn and Pb in high purity copper using ICP-MS has been investigated. One gram of sample was dissolved with 8ml of 7 M nitric acid. After lanthanum solution (La: 10 mg) was added, the pH of the sample solution was adjusted to 910 with 0.3 M ammonia water and As, Sb, Bi, Sn and Pb ions were coprecipitated with lanthanum ion as their hydroxides. After filtration, the precipite was dissolved with hot nitric acid and diluted to 20 ml with water. As, Sb, Bi, Sn and Pb were determined by ICP-MS. The respective detection limits were 0.04 (As), 0.01 (Sb), 0.008 (Bi), 0.01 (Sn) and 0.02 (Pb) ng ml-1 and the relative standard deviations were less than 2.5% at 100 ng of analyte.View full abstractDownload PDF (680K) -
Kuniaki KAWATA, Fumio SHIRAI1990 Volume 39 Issue 1 Pages T23-T28
Published: January 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSRound robin tests were carried out to investigate the precision of determinations of low molecular weight halogenated hydrocarbons in waste water by two methods prescribed in JIS K 0125. Three samples of waste waters with added trichloroethylene, tetrachloroethylene and 1, 1, 1-trichloroethane were analyzed by 12 laboratories. The results showed that the precision of the solvent extraction/GC method was better than that of the head-space GC method; there were no significant differences between the means obtained by the two methods.View full abstractDownload PDF (880K)
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