All issues
Volume 39, Issue 6
Displaying 1-14 of 14 articles from this issue
- |<
- <
- 1
- >
- >|
-
Masao UMEMOTO, Koji HAYASHI1990 Volume 39 Issue 6 Pages 317-321
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe ICP-AES utilizing graphite cup direct insertion technique was investigated for the determination of trace elements in human hair. The graphite cup used was characterized by a large volume capacity of 50μl, a cup wall thickness of 0.5 mm and a slender rod of 1 mm in diameter. A sample volume of 25μl was applied to obtain higher sensitivity. Compromised optimum operating conditions were studied in order to attain higher precision and lower detection limits as well as to eliminate matrix effects on the volatilization of sample and memory effects. The graphite cup direct insertion technique was applied to the analysis of Cd, Pb, Cr and Ni in the certified reference material (NIES No. 5) and the results agreed well with the certified values. This method was confirmed to be applicable to samples containing Ca and Al as major elements.View full abstractDownload PDF (642K) -
Kazuo UCHIKURA1990 Volume 39 Issue 6 Pages 323-326
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA selective and sensitive method for the determination of oxalic acid using the electrogenerated chemiluminescence (CL) system, oxalate-Ru(bpy)32+, was described. Oxalate was reacted with Ru(bpy)33+ continuously prepared from Ru(bpy)33+ with an electrochemical reactor (ECR, home-made). The dual channel FIA apparatus was comprised of a delivery pump for both carrier and reagent solutions, a sample injector, damper tubing, the ECR and a photon counter. The oxidation potential of the working electrode in the ECR was maintained with a potentio-galvanostat. CL intensity was measured with a photon-counter which recorded FIA peaks graphically. The carrier solvent was H2O (flow rate, 0.3 ml/min-1) and reagent solution prepared in 10 mM H2SO4 to contain 0.12 mM Ru(bpy)3Cl2 (flow rate, 0.8 ml min-1). The sample (10 μl) was injected into the carrier stream. Linearity was obtained up to 16 pmol for oxalate. The detection limit was 0.3 pmol (S/N=3). The relative standard deviation was 2.3% (n=5, 5 pmol). This method was successfully applied to the determination of oxalate in urine.View full abstractDownload PDF (470K) -
Munehiko MIZOBUCHI, Kunitoshi ICHIMURA, Susumu TOMITA1990 Volume 39 Issue 6 Pages 327-331
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIon chromatography is useful for the determination of anion species in environmental waters such as river-, treated waste- and mineral spring-water. Usually it is difficult to separate and determine fluoride in samples containing acetic and formic acids. Then, the authors tried to develop a new analytical method to separate acetate and formate ions from fluoride and chloride ions. The step gradient method with sodium hydroxide solution as an eluent was used to separate those anion species. Recoveries of fluoride ion were 92 to 108% for river-, treated waste- and mineral spring-water. The results obtained by the proposed method were compared with those obtained by JIS method and an isocratic method with carbonate and bicarbonate as an eluent. Although the isocratic method gave higher concentrations than those obtained by the standard JIS method, the results obtained by the proposed method showed almost the same results as the JIS method. The proposed gradient method can be useful for the determination of fluoride ion, especially for the treated waste water.View full abstractDownload PDF (615K) -
Ion-solvent interactions in acetylacetone VIIIIkko SAKAMOTO, Satoshi OKAZAKI1990 Volume 39 Issue 6 Pages 333-340
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe complex formation constants of sodium ion in acetylacetone (2, 4-pentanedione, Hacac) with other solvents have been determined at 298 K by potentiometry using a sodium ion-sensitive glass electrode. The complexing solvents used were acetonitrile (AN), acetone (AC), water, methanol (MeOH), ethanol (EtOH), N, N-dimethylformamide (DMF), N, N-dimethylacetamide (DMA) and dimethyl sulfoxide (DMSO). The Gibbs free energies of transfer of sodium ion from Hacac to these solvents have also been determined assuming the liquid junction potential as negligible. The stability of sodium ion increases, in general, with solvent basicity in the following order: Hacac<AN, EtOH<AC, MeOH<water<DMF<DMA, DMSO. As for complex forming, only one solvent molecule of AN and MeOH solvated the sodium ion in Hacac. Mono- and di-solvated sodium ions were formed for AC, water and EtOH. Tri-solvated species were also detected for DMF, DMA and DMSO. In general, the degree of complexing of the sodium ion increases with solvent basicity. The quantitative correlation between the sodium ion-solvent complexing and the ion transfer is discussed on the basis of the coordination model of ionic solvation.View full abstractDownload PDF (968K) -
Akihiro NAMBA, Hirobumi SUZUKI, Atsuo MIYAKAWA, Toshimitsu MUSHA1990 Volume 39 Issue 6 Pages 341-345
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIntensity fluctuations of laser light scattered by suspended latex spheres in water were measured. The power spectral density showed the Lorentzian form. The particle size of the latex spheres could be estimated from the relaxation frequency. The dependency of relaxation frequency on particle size was applied to an immunoassay of IgE. Latex sphere particles coated with an antibody agglutinated through immunoreaction and, as a result, the shape of power spectra changed. The change of the particle size was estimated from the relaxation frequency. The ratio of the relaxation frequency between the original and the reacted sample was measured as a function of IgE antigen concentrations. The IgE antigen of 0.1 IU/ml could be detected by this method.View full abstractDownload PDF (673K) -
Junichi KOYAMA, Junko NOMURA, Okitsugu NAKATA, Masahiro MATSUOKA1990 Volume 39 Issue 6 Pages 347-351
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSimultaneous determination of vanillylmandelic acid (VMA), homovanillic acid (HVA) and creatinine (Cre) in urine has been studied by HPLC. The separation of VMA and HVA from other components in urine was achieved by the ion-pair mode at pH 3.75. However, Cre was not retained under this condition, and required a higher pH (>6) for it to be retained. Thus these three materials could not be analyzed under the same conditions. However, the column-switching technique has made it possible to determine them simultaneously. By using this method, VMA, HVA and Cre in urine were determined simultaneously within 25 min. The amount of Cre determined by this method corresponded to that obtained by the Jaffe method.View full abstractDownload PDF (443K) -
Naoko SHIBATA, Noriko FUDAGAWA, Masaaki KUBOTA1990 Volume 39 Issue 6 Pages 353-358
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSignal profiles of rare earth elements (REEs) observed as the signal-time curves were investigated by inductively coupled plasma mass spectrometry (ICP-MS) using a tungsten (W) boat electrothermal vaporization (ETV) device as a sample introduction system. Twentymicroliters of REE standard solutions applied on the W-boat were heated to produce the profiles. Both the Ar-H2 carrier gas flow rates supplied into the glass chamber and the heating temperature of the W-boat influenced the profiles. Increasing the gas flow rates resulted in a delayed peak time. Decreasing the heating temperature gave a flat profile with a small peak and caused a memory effect on the W-boat. Signal appearance times and the peak times of REEs were later than those of common metals such as Pb and Co. This suggests that REEs are not easily vaporized on the W-boat. REEs which have higher melting points showed profiles with later peak times and more significant memory effects. These results indicate that the signal profiles of REEs are dependent on the melting points of the elements.View full abstractDownload PDF (602K) -
Koji YAMAGAKI, Tadashi TAKAHASHI, Keio YAMADA, Michinao YOSHII1990 Volume 39 Issue 6 Pages 359-361
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSelenium in 500 ml of water sample acidified with 25 ml of 12 M HCl was reduced to its hydride by addition of 45 ml of 30% sodium tetrahydroborate solution. Volatile hydrogen selenide formed was absorbed into 5 ml of the solution adjusted to pH 11 with NH4OH. Selenium in the absorbing solution was determined by ICP-AES. Cu, Bi, Ag and As ions interfered with hydride generation of selenium. The recovery of selenium by this method was 93% and the analytical results of river water were in good agreement with those obtained by spectrophotometry. The relative standard deviation was 4.1%. The detection limit was 0.5 μg/l for 500 ml of water sample.View full abstractDownload PDF (315K) -
Kunishige HIGASHI, Akinori KAWAHARA, Shin-ichi WAKIDA, Masataka YAMANE ...1990 Volume 39 Issue 6 Pages 363-365
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn apparatus was developed for automatic measurement and to evaluate the pattern of molecular weight distribution of organic substances dissolved in water. A separation column (7.6 mm i.d., 25 mm in length) packed with Asahipak GS-220 was used. Distilled water was used as the mobile phase at flow rate of 1 ml/min, and a chromatogram was obtained by a high sensitive refractive index detector. The apparatus was regulated automatically by a system-controller. Sample size necessary for an analysis was 0.5 ml of filtrated environmental water without preconcentration, and one chromatogram was obtained in twenty minutes. Some enviromental water gave different chromatographic patterns. River water was measured by the apparatus continuously and automatically and chromatograms were obtained once an hour, which showed the change of the patterns from morning to evening. The apparatus was found to be suitable for an automatic measurement of organic substances dissolved in enviromental waters.View full abstractDownload PDF (275K) -
Chao-Long LI, Tomokazu TANAKA, Hiroshi KAWAGUCHI1990 Volume 39 Issue 6 Pages 367-369
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA vertical, cone-type spray chamber with a capacity of ca. 52 ml was constructed to reduce the memory effect in ICP-AES. A concentric glass nebulizer was placed at an angle of 10° to the horizontal near the bottom of the chamber along with a glass-bead spoiler. The decrease of the intensity of a manganese line for the 1000 μg ml-1 Mn solution was measured after the sample was changed to deionized water. It took 40 to 50 s to reduce the intensity to that equivalent to 0.1 μg ml-1, while 22.5 min was necessary with a Scott-type spray chamber. Signal-to-background ratios and detection limits for various elements with the present spray chamber were comparable or superior to those for the Scott type except for lanthanum.View full abstractDownload PDF (324K) -
Ryoichi KIZU, Motoichi MIYAZAKI1990 Volume 39 Issue 6 Pages 371-374
Published: June 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe novel aspects of Cisplatin, a potent antitumor platinum complex, on HPLC with ion exchange columns were studied. Although Cisplatin is an inorganic nonionic complex, it was retained on both anion and cation exchange columns, but not on reversed-phase columns. The capacity factor was larger on a column with higher ion exchange capacity; a capacity factor of more than 30 was obtained in a system composed of anion exchange MCI GEL CA 10S column and sodium dihydrogen phosphate eluent. However, the capacity factor measured on a column using the appropriate salt solution as the eluent was not affected by changing the concentration or pH of the eluent. The effect of UV absorptivity of an eluent on the peak height of Cisplatin was studied at various wavelengths in order to confirm the absence of an ion-exchange sorption mechanism in the eluent. No difference was observed between the relative peak height-detection wavelength profiles obtained with UV absorbing eluents and those obtained with UV-non absorbing eluents. These results indicated that Cisplatin might not be retained by ion exchange mechanism, but by other mechanisms such as ion-dipole interactions between Cisplatin and the functional groups of the stationary phases.View full abstractDownload PDF (518K) -
Takashi WATANABE1990 Volume 39 Issue 6 Pages T77-T81
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSoil fumigants such as chloropicrin (CP) and dichloropropene (DCP) have such high vapor pressure that they are easily volatilize into atmosphere. In order to monitor the air contamination caused by the soil fumigants, the effective method for trapping them was investigated. The break-through volumes (BTV) were measured to evaluate the efficiency of 10 adsorbents for trapping them in the air. Porapak series generally had larger BTV than the other adsorbents. The BTV of Porapaks had a range from 100 to 1000l/g, and particularly T type showed a BTV with more than 2500 l/g. The BTV of the other adsorbents was only less than 20 l/g. The stability of the fumigants on Porapak Q, R and T was measured. The fumigants on Porapak Q proved to be the most stable, and the stability on Porapak T was slightly inferior to that on Porapak Q. The recovery efficiencies from Porapak T treated with 0.5250 ng of CP, 10250 ng of DCP (Z), and 10500 ng of DCP (E) in 10 l of the air showed over 80%. And the recovery of CP and DCP from Porapak T showed over 80% when applied at 110 μg in 1 l of the air, while that from Porapak Q was below 50% at any conditions. Although the fumigants are slightly unstable on Porapak T, the unstability seemed to have no serious effect on practical analyses. Therefore, Porapak T (0.2 g) can be used as the most suitable adsorbent for trapping those fumigants at concentration level of 0.05 μg/m310 mg/m3 for CP and 1 μg/m310mg/m3 for DCP.View full abstractDownload PDF (676K) -
Hiroyasu YOSHIKAWA, Youichi ISHIBASHI, Naoki GUNJI, Kouichi SASAYAMA, ...1990 Volume 39 Issue 6 Pages T83-T87
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe retention behavior of 38 elements on mini-column iminodiacetate type chelating resin (0.5 cm3) was investigated by using ICP-AES or AAS. Divalent ions, their oxocompounds and some trivalent ions could be recovered from this mini-column after the adsorption. For the simultaneous recovery of these elements, the adsorption and elution were carried out at pH 4 and 9 M nitric acid, respectively. On the other hands, monovalent ions and their oxocompounds could not be retained on this chelating resin. Twenty one elements (Al, Ba, Ca, Ni, Pb, U, Th etc.) in high purity silica, silicon nitride and silicon carbide were determined by ICP-AES after separation with this mini-column chelating resin. The lower detection limit of each element in high purity silica and silicon nitrde showed nearly same values, but in the case of silicon carbide, these values were higher due to the complexity of its analytical procedure.View full abstractDownload PDF (566K) -
Michio ZENKI, Toshiyuki ITOH, Kyoji TÔEI1990 Volume 39 Issue 6 Pages T89-T92
Published: June 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAn application of HPLC to the determination of fumaric acid in commercially available malic acids and apple drinks was examined. The fumaric acid was separated on a TSK-gel 120A column (ODS C18, 4.6 mm i.d.×150 mm) with an eluent of 0.1 M sodium perchlorate-0.01 M sodium dihydrogenphosphate (pH 2.6). The eluate was monitored with a UV detector at 210 nm. The sensitivity of the fumaric acid was quite good and sufficient separation could be achieved within 10 min. The calibration curve between peak area and fumaric acid concentration was linear up to 2.0×10-5 M. Recoveries of fumaric acid in malic acids and apple drinks were in the range of 98105% with good reproducibilities (R. S. D., less than 1.5%). Fumaric acid in eighteen commercially available samples (D-, L- and DL- malic acids and apple drinks) were determined successfully by the proposed method.View full abstractDownload PDF (529K)
- |<
- <
- 1
- >
- >|