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Volume 41, Issue 4
Displaying 1-12 of 12 articles from this issue
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Mikita ISHII, Masatoshi MIURA, Jun SATO1992 Volume 41 Issue 4 Pages 157-162
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSuccessive determination of hydrogen sulfide and sulfur dioxide in the atmosphere was investigated by using a flow-type analyzer equipped with a chemiluminescent (CL) detection system for the CL of excited sulfur dioxide by the oxidation with potassium permanganate. The analyzer is comprised of three flow lines. The sample flow line with a trap system for sulfur dioxide and hydrogen sulfide was operated at a flow rate of 10 ml/min and the two reagent flow lines supplying the 4×10-6 M potassium permanganate solution and the 4×10-3 M riboflavine phosphate solution were operated at a flow rate of 3.0 ml/min. The lower detection limit was 1.78×10-7 M for sulfur dioxide and 8.92×10-7 M for hydrogen sulfide and the relative standard deviation was 4.0% for 3 repeated runs of the 2.23×10-6 M sulfur dioxide solutions and 3.6% for the 2.23×10-6 M hydrogen sulfide solutions. Sodium thiosulfate alone gave the CL response as large as that of hydrogen sulfide in the CL reaction. The results obtained by the proposed method agreed well with those by the conventional method.View full abstractDownload PDF (881K) -
Shogo SUZUKI, Shoji HIRAI1992 Volume 41 Issue 4 Pages 163-166
Published: April 05, 1992
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMultielements in NIES (National Institute for Environmental Studies of Japan) certified reference material No. 12 marine sediment were determined by instrumental neutron activation analysis (INAA). Six portions of the marine sediment reference material (ca. 50430 mg) were irradiated successively, at first for a short time (30 s) at a thermal neutron flux of 1.5×1012n cm-2 s-1 and then for a long time (12 h) at a thermal neutron flux of 1.7×1012n cm-2 s-1 in the Rikkyo University Research Reactor. After a suitable decay-period, these irradiated portions were measured by three γ-ray spectrometric methods; a conventional counting method using a coaxial Ge detector, and an anticoincidence and a coincidence counting method 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. Corrections for overlapping interference peaks and interfering nuclear reactions were applied to the spectral data. Concentrations of 54 elements (Na, Mg, Al, Si, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Br, Rb, Sr, Zr, Mo, Ag, Cd, In, Sn, Sb, I, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Au, Hg, Th, U) were determined by these counting methods.View full abstractDownload PDF (492K) -
Yoshiaki SASAKI, Shoji TAGASHIRA, Yoshiko MURAKAMI, Isamu FUJIWARA, Ya ...1992 Volume 41 Issue 4 Pages 167-172
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAdsorption of silver ion by freshly precipitated silver chloride could be represented by the following two types of expressions, (A)pAg+ads.=apAg-c, and (B) Ag+ads=K-bpAg, in the pAg range of 3.6 to 4.8, where Ag+ads.is amount of adsorbed silver ion, Ag is the equilibrium concentration of silver ion, and others are constants. On the other hand, in the case of adsorption of silver ion by powdered silver iodide, the plot of Ag+ads. against pAg gave two regression lines in 2×10-3 mol dm-3 HNO3 medium and three in 1.8×10-2 mol dm-3 H2SO4 medium in the pAg range of 3.0 to 6.4. By applying the type (A) expression, however, we could obtain only one regression line in the same pAg region. This indicates that adsorption of silver ion by silver halides followed a Freundlich equation over a wide pAg region.View full abstractDownload PDF (647K) -
Sadayuki SATOH1992 Volume 41 Issue 4 Pages 173-178
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPyrolysis-derivatization-gas chromatography developed by J. M. Challinor was applied for the identification of copolyester formed from p-hydroxy benzoic acid and 2-hydroxy-6-naphthoic acid. By the proposed method of adding the alkylating reagent (tetramethyl ammonium hydroxide) to the polymer sample before pyrolysis, the derivatization efficiency was not high enough. Therefore, some modifications were made to attain optimum conditions. The quantitative derivatization of the pyrolysis products was able to get by introducing the reagent into the pyrolyzer during the pyrolysis. This modified method was applied to identify various synthetic polymers. The derivatization mechanism during pyrolysis was also discussed.View full abstractDownload PDF (824K) -
Hideaki KINOSHITA, Tokuji IKEDA, Shinji KOGA, Sakayu SHIMIZU, Hideaki ...1992 Volume 41 Issue 4 Pages 179-183
Published: April 05, 1992
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNucleoside oxidase was purified to homogeneity from cells of Flavobacterium meningosepticum. This enzyme was immobilized onto the surface of a graphite paste electrode containing benzoquinone and the enzyme layer was covered with dialysis membrane. This enzyme electrode produced a biocatalytic anodic current in the presence of nucleosides in buffer solutions of pH 610. The electrode showed a higher current response to nucleosides containing the purine bases, adenosine, guanosine and inosine, compared with those containing the pyrimidine bases, uridine, cytidine and thymidine. The sensitivity to the latter was 80% of that to the former. A linear relationship was obtained between the current and the concentration of nucleosides ranging from 2 to 30 μM. This electrode did not respond to bases, sugars and nucleotides. The activity of 5'-nucleotidase in serum could be easily assayed using the present electrode in the presence of nucleotides.View full abstractDownload PDF (626K) -
Masayuki NISHIMURA, Morimasa HAYASHI1992 Volume 41 Issue 4 Pages 185-189
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetector response in ion chromatography is normally given as a function of the difference in ion-equivalent electroconductivity between an analyte ion and a competing ion, since the elution of the analyte ion is accompanied by a decrease in the concentration of the competing ion equivalent to that of the analyte ion. If the elution of analyte ions and the changes in concentration of the competing ion could be monitored separately, chromatographic results would include qualitative information, since the peak area of an analyte ion is not only dependent upon concentration but is also dependent upon ion-equivalency and thus can be used as an identifier. In this study, we tried to resolve peak components into the analyte ion and the competing ion by means of a second column following the analytical column, through which they migrate at different speeds. When a reversed-phase chromatographic column (Asahipak GS-310M) was used as the second column, each anion that was separated on the analytical column {Shim-pack IC-A3, mobile phase, 2.5 mM phthalic acid and 2.4 mM tris(hydroxymethyl)aminomethane} gave two peaks; one positive and the other negative. The areas of the positive peaks were peculiar to the individual anions corresponding to electroconductivities, while the areas of negative peaks were essentially equivalent to analyte concentrations. The anions, therefore, could easily be identified by using the ratios of positive and negative peak-areas along with retention times.View full abstractDownload PDF (578K) -
Futoshi YOSHIMURA, Takehiko SUZUKI, Masaaki YAMADA, Toshiyuki HOBO1992 Volume 41 Issue 4 Pages 191-196
Published: April 05, 1992
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA catalyst-immobilized ion-exchange resin as the indicator phase of a flow-through chemiluminescence(CL) sensor is described. Adrenaline CL was chosen as a model CL system, the light emission resulting from the aerobic oxidation of adrenaline in alkaline solution containing ordered surfactant assemblies and manganese(II) ion catalyst. The sensor consisted of a Pyrex tube (26 mm×5 mm i.d.) packed with manganese catalyst-immobilized anion-exchange resin as the indicator phase and a photomultiplier tube. Anion-exchange resins (OH- form) themselves functioned as favorable reaction media for the adrenaline CL reaction;in particular, a strongly basic resin (Amberlite IRA-410) provided a CL signal 100 times stronger than a nonionic resin (Amberlite XAD-2). Further, a 7.5-fold increase in the CL signal was observed with manganese(III)-tetrakis(4-sulfonatophenyl)porphyrin immobilized on the IRA-410 resin as a catalyst. This indicator phase permitted adrenaline to be detected down to 3×10-6 M with a 20-μl injection into a water carrier without special regard for the selection of resin, the sensor geometry, and the experimental conditions. The relative standard deviation (n=10) was 3.5% for 5×10-5 M adrenaline. Successive injections of adrenaline caused gradual deterioration of the indicator phase (after 60 injections of 5×10-5 M adrenaline there was a 10% decrease in the CL signal), but its regeneration was readily accomplished by passing 1 M NaOH solution through the sensor. The sensor was successfully applied to determine adrenaline in a drug sample.View full abstractDownload PDF (739K) -
Munehiko MIZOBUCHI, Yukiko HORIE, Kazuo SAITO1992 Volume 41 Issue 4 Pages 197-201
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIon chromatography with a UV/VIS-detector set at 370 nm was used to determine chromate ion extracted from industrial waste materials in an alkaline solution. Since chromate ion could not be detected by the JIS method because of its reduction by unknown chemical species in the materials, this method was useful in the detection without any effect from other anion species. The detection limit of this method was 0.3 mg/l and recoveries were from 95.0% to 104%. Chromate ion could be detected at the concentration of 0.4 mg/l in the solution prepared from industrial wastes.View full abstractDownload PDF (537K) -
Kenji SATO, Kosaku HARADA, Shigeyuki TANAKA1992 Volume 41 Issue 4 Pages 203-205
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPretreatment procedure of sample was investigated in the ion chromatographic determination of total Mg and Ca in milk. Nitric acid was a better solvent than the other solutions, such as trichloroacetic acid, EDTA and hydrochloric acid, for the extraction of total Mg and Ca from milk. The recommended procedure was as follow: milk sample was diluted five times with distilled water. An aliquot (1.5 ml) of the sample solution and 3.5 ml of 1 M nitric acid were pipetted into a glass tube. After mixing, centrifuging, and filtration with membrane filter, a 100 μl aliquot was analyzed with a precolumn (Shodex Y-521P, 10 mm×4.6 mm i.d.) and a separation column (Shodex Y-521, 150 mm×4.6 mm i.d.). A solution containing 2 mM ethylenediamine and 4 mM tartaric acid was used as a mobile phase (1 ml/min). The detection limits (S/N=3) of the proposed method for Mg and Ca were 30 ppb and 70 ppb, respectively. Relative standard deviation (n=7) was less than 1% for the simultaneous determination of Mg and Ca. The values obtained by the proposed method for Mg and Ca in the milk samples (n=6) were 109118 ppm and 11201190 ppm, respectively, which agreed well with those by the AAS method.View full abstractDownload PDF (351K) -
1992 Volume 41 Issue 4 Pages e1
Published: 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (55K) -
Akio MASUI, Kiyoshi YAMAMOTO, Koji OHTA1992 Volume 41 Issue 4 Pages T49-T54
Published: April 05, 1992
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe actual penetration depth of the electric field (dp) in attenuated total reflection-IR (ATR-IR) spectroscopy has been calculated for the diethyleneglycol-bis-allylcarbonate (CR39) polymer from its optical constants. The frequency dependence of the dp is discussed in relation to the frequency dependence of the optical constants as well as the ATR-IR spectra calculated using the Fresnel equations. The maximum and the minimum dp respectively occur at frequencies just below and above the frequency of the ATR-IR peak, which can be called the dp anomaly. The actual dp is compared in detail with the dp of the evanescent wave, which is often used as an approximation for penetration in weakly absorbing samples. The way that refracted light energy at the absorbing frequency regions is transmitted along the z direction is also discussed. It is concluded that when the refractive index of the prism and/or the angle of incidence is relatively small, care must be taken in interpreting the ATR-IR spectral shape concerning the dp anomaly for samples which are heterogeneous along the z direction. In addition, the interference fringes might be expected to appear exclusively at frequencies just below the ATR peaks for thin film samples.View full abstractDownload PDF (682K) -
Hiromasa KATOH, Hiroko FUJINO, Akiyoshi NOZAWA1992 Volume 41 Issue 4 Pages T55-T58
Published: April 05, 1992
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the determination of water content in polymers, we compared the heating vaporization-Karl Fischer (KF) coulometric titration method with the official standard method in which a polymer sample is completely dissolved in an appropriate solvent before an aliquot is taken for KF volumetric titration. Compared with the latter standard currently in use, the former method has the following merits; simple operation, lower determination limit and good reproducibility. Thus it is considered suitable as an official method.View full abstractDownload PDF (382K)
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