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Volume 40, Issue 4
Displaying 1-14 of 14 articles from this issue
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Sadaaki MORIGUCHI, Kunishige NAITO, Shinsuke TAKEI1991 Volume 40 Issue 4 Pages 153-158
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSNew packings for gas chromatography were prepared using the following procedure: first Chromosorb G NAW was coated with a desired amount of ethylene dimethacrylate (EDMA) as a monomer and α, α'-azobisisobutylonitrile as an initiator for polymerization (1 to 20% of the coated amount of EDMA). Polymerization of EDMA was carried out in an atmosphere of nitrogen at 80°C. The packing was washed for 6h with methanol and dried at 60°C under vacuum for 3h prior to use. The packing prepared by this procedure was stable up to approximately 200°C. The retention volume of some aliphatic alcohols with 1 to 4 carbon atoms increased in a nonlinear rate when the polymer content of the packing was increased. This result suggests that at least two or more sorption equilibria take part in the retention of the solutes. On the assumption that partition into a polymer layer and adsorption on the polymer layer concurrently contributed to the retention of the solutes, the retention volume of each solute was analyzed according to the procedure of Martin et al. Through this analysis of experimental data, it was demonstrated that the partition equilibrium was more significant than the adsorption equilibrium in the retention of the solute, especially for aliphatic alcohols. From this result, it was concluded that the EDMA-polymer layer formed on Chromosorb G NAW showed a stronger affinity for polar alcohol molecules than for non-polar hydrocarbonmolecules.View full abstractDownload PDF (528K) -
Yasuo HAYASHI, Kiyoshi MATSUMOTO1991 Volume 40 Issue 4 Pages 159-162
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAnalysis of oxide/metal interface using SIMS has been investigated. In general, SIMS enables us to detect trace amounts of elements, but the change of the secondary ion yield at the interfaces results in ghost peaks during the depth profile analysis. This phenomenon makes it difficult to get accurate information on interdiffusion at the multilayer interface. In this study, use of Cs+ primary beam with detection of CsX+ cluster ions has been found to successfully eliminate those ghost peaks, since CsX+ cluster ions are free from matrix effects. The developed technique was used to analyze Si/ZnO and TiN/glass interfaces. Mechanisms with respect to bonding properties and stability of the coating films are discussed on the basis of this analysis.View full abstractDownload PDF (500K) -
Toshihiro SHIRASAKI, Akira YONETANI, Kouichi UCHINO, Kaoru SAKAI1991 Volume 40 Issue 4 Pages 163-168
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSBy using a graphite tube treated with molybdenum, the optimum conditions for the determination of gallium by AAS have been investigated. The procedure for molybdenum-coating was as follows: A pyrolytic graphite tube was mounted in an atomizer unit. Twenty microliters of ammonium molybdate solution (500μg/ml) was injected into the tube. The tube was heated in a ramp mode from 80°C to 120°C for 25 s, from 120°C to 150°C for 30s, then in a step mode from 1000°C for 30 s and finally at 3000°C for 5s. This reagent-addition and heating procedure was repeated ten times. Sulfuric acid, hydrochloric acid and perchloric acid showed suppression effect on the absorbance of gallium, while nitric acid did not show a significant suppression effect until it reached a concentration of 3.0M. The sensitivity of this method using the molybdenum-treated graphite tubes was thirty times higher than when using normal pyrolytic tubes. The proposed method was applied to the determination of gallium in Orchard Leaves (NIST SRM 1517) and Pond Sediment (NIES No.2). The analytical results were in good agreement with the reported values. One percent absorption of gallium of this method was 1.1ng/ml. The relative standard deviation was approximately 4% (n=90).View full abstractDownload PDF (3222K) -
Tokishi HAYASHI, Chiaki IKEURA, Hidemi TODORIKI1991 Volume 40 Issue 4 Pages 169-173
Published: April 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA reliable method was developed for the determination of 3-carboxy-4-methyl-5-propyl 2-furanpropionic acid (CMPFPA) in human plasma. In the course of preliminary experiments, it was found that use of methylation with diazomethane after solvent extraction simplified the sample preparation. The HPLC was equipped with a UV detector. However, detection sensitivity was not high enough because of low absorptivity. Therefore, further investigations were carried out so that a larger volume of the sample solution could be injected into the HPLC. Two hundred microliters of human plasma were mixed with 800 of 2-propanol containing 50ng of anthracene-9-carboxylic acid (ACA) and centrifuged. The supernatant was evaporated to dryness. The residue was redissolved with 2ml of 0.1M phosphate buffer (pH7.0) and washed twice with 5ml of hexane each by shaking for 5min. CMPFPA was extracted twice with 7ml of ethyl acetate each after addition of 0.5ml of 1.0M HCl and 0.7g of NaCl. The organic layer was evaporated to dryness after being dried over Na2SO4. The residue was dissolved with 1ml of ethanol and mixed with 0.5ml of a diazomethane solution in ether. After allowing to stand at the room temperature for 15min, the mixture was evaporated to dryness. The residue was carefully redissolved with 150μl of ethanol anddiluted with 225μl of redistilled water. One hundred and fifty microliters of the resulting solution were injected into HPLC. The separation was carried out with a stainless-steel column (250mm×4mm i.d.) packed with LiChrosorbR RP-8 (5μm) and 60% aqueous acetonitrile solution as a mobile phase (1ml/min). A UV monitor (254nm) was used for monitoring. This simple method showed good reproducibility (n=11, SD=1.36% ). The method was also used for the determination of plasma CMPFPA on healthy volunteers.View full abstractDownload PDF (561K) -
Kazuhisa MORIYASU, Hidenobu MIZUTA, Yasuharu NISHIKAWA1991 Volume 40 Issue 4 Pages 175-179
Published: April 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA XRF method for the simultaneous determination of scandium(III), yttrium(III) and lanthanoid(III) ions in minerals was established. The rare earth minerals, monazite and xenotime, are treated with conc. H2SO4. Thortveitite having a major constituent of scandium silicate is treated with HF and KHSO4. The rare earth metal ions in the solution are precipitated with oxalic acid. Then the precipitates are filtered and ignited to give the rare earth oxides. The oxides are dissolved in conc. HCl. The definite amount of sample solution (pH4) is added to HIDA-resin which is prepared by chemical bonding of imminodi acetic acid derivatives on an aminostyrene-divinylbenzene copolymer, and then metal-HIDA chelates are formed. After the resin is dried, fifteen fold of cellulose powder is added to the definite amount of resin. The homogenized mixture is pressed to form a pellet (thickness: 1-2mm, diameter: 40mm). Contents of rare earth ions in the pellet is determined by XRF spectra. Mixed solution of multiple rare earths are prepared to have comparable composition as minerals, XRF spectra of them are measured according to the above procedures. The analytical results of rare earth ions in minerals by the present method were agreed with that of ICP-AES method within 10% deviation. This method is useful for rapid determination of multielement rare earths.View full abstractDownload PDF (496K) -
Daijiro YAMAMOTO, Masamichi TSUKADA, Daiei SATO1991 Volume 40 Issue 4 Pages 181-186
Published: April 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of ethanol in liquors using erythrosine lactone was examined. Erythrosine was extracted from acidic solution into hydrophobic organic solvents as a colorless species of lactone type. An orange color was developed by the addition of a small quantity of alcohol into the extract. When this solution was mixed with water, the color was distributed into both phases, the water and the organic solvent. Photometric measurement was carried out using the water phase to determine the content of ethanol. This method had two weak points. One was lack of reproducibility owing to the temperature dependence of the distribution. The other was that this method was not able to be applied to colored liquors. Another method was investigated. When an aqueous solution of approximately 2M HCl was added to the liquor phase, colored species of erythrosine remained in the organic phase. Photometric determination was performed by using the organic solvent phase. By this method the ethanol content of colored liquors was determined without distilling. The analytical results on some liquors agree well with the labeled values on bottles.View full abstractDownload PDF (646K) -
Masahiko IKEDA, Hiroshi UCHIHARA, Masatoshi OSAWA1991 Volume 40 Issue 4 Pages 187-191
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSInfrared absorption of thin organic films is enhanced extremely by undercoating with silver island-films. The fundamental properties and mechanisms of this phenomenon, and application to trace analysis are discussed. The silver films of 5-20nm in mass thickness (dAg) were vacuum evaporated on CaF2 plates. Several monolayers of p-nitrobenzoic acid were deposited onto the Ag films. The IR spectra were obtained using conventional transmission method. The symmetric modes of the first monolayer chemisorbed on Ag were enhanced selectively. The absorption intensity increased with increasing dAg and became maximal at approximatry dAg=10nm. The enhancement factor for the chemisorbed molecules was estimated to be ca. 300 under the optium conditions. The enhancement was much less on quasi-continuum Ag films of dAg>13nm. The effect arises mainly from the amplification of the incident IR. field through the collective electron resonances (plasma oscillations) of aggregated Ag islands. Some minor chemical contribution to the enhancement is also proposed. The infrared measurement using this surface-enhanced phenomenon has potential as a new trace analytical technique.View full abstractDownload PDF (614K) -
Effect of anodic pretreatment of glassy carbon electrodes on electrochemical detection of denopamineKazuya YAMASAKI, Masahiro YASUDA, Yoshio KOKUSENYA, Masaaki MATSUO1991 Volume 40 Issue 4 Pages 193-197
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAnodically pretreated glassy carbon (GC) electrode was used in the electrochemical detection of denopamine (DP). The optimum condition for the pretreatment of the GC electrode was attained by anodic oxidation in 0.1M acetate buffer containing 2mM tetrabutylammonium bromide (pH 6.2) at+1.6V vs. SCE for 10min, followed by cathodic reduction in the same solution at -1.0V vs. SCE within a second. By this treatment, an approximate 9 fold increase was obtained in the peak current (IP). This increase was proportional to the concentration of DP from 0.1 to 1.5mM. The treated GC electrode gave reproducible IP with a relative standard deviation of 3.9% (n=6). The effect of this treatment was presumably due to the acceleration of oxidative reaction of DP with tertiary ammonium bromide which was incorporated to the surface film created in oxidation of acetic acid. The same treatment effect was observed in the other drug analysis.View full abstractDownload PDF (527K) -
Satoshi KAWAI, Mika NOGUCHI, Chieko ISHIGURE, Kyoko KODAMA1991 Volume 40 Issue 4 Pages 199-202
Published: April 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSColor reactions of 36 homovanillic acid related compounds were examined using threekinds of nitrosonaphthols, 1-nitroso-2-naphthol, 2-nitroso-1-naphthol and 2-nitroso-1-naphthol-4-sulfonic acid. Reaction specificity is discussed. Guaiacols, phenols with an electron donating group para to the hydroxyl and 5-hydroxyindoles gave generally positive reaction, while compounds having strongly electron-withdrawing groups resulted in no coloration. Catechol derivatives also gave no coloration. Differences were observed in color intensity of some compounds when acetic acid and ethanol were used as the solvent. However, the three reagents resulted in slight variations.View full abstractDownload PDF (325K) -
Kunio NAGASHIMA, Ichiro YAJIMA, Toshiyuki HOBO1991 Volume 40 Issue 4 Pages T77-T81
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn Au-poly(ethylene oxide)4.5AgCF3SO3-Ag galvanic gas detector, consisting of a disc (13mm in diameter×1.1mm thick) has been developed by utilizing a polymeric electrolyte film (30μm thick). The polymeric films were made by mixing acetonitrile solution with both AgCF3SO3 and polyethylene oxide. The mixture was cast on the disc and the solvent was permitted to evaporate. The working electrode (25nm thick) was made by coating it with vaporized gold. The maximum response appeared within 3 s after the sample (2.6ml) was injected into the nitrogen carrier stream. The flow rate was 40ml min-1. The longest time to return to the base line was 3 min. The maximum current flowing in the external circuit increased linearly relating to the concentration of NO2 in the range 0.28ppm at ambient temperature. Twenty samples could be analyzed per hour. The relative standard deviation of the response for 1.0ppm of NO2 using 2.6ml sample was about 3%. After 200 samples (1ppm of NO2-2.6ml) had been analyzed, the response decreased by about 15% of its original value.View full abstractDownload PDF (561K) -
Eiko SHIMADA, Jun ISHIGOOKA, Sadanori MIURA, Hiroaki KUBO1991 Volume 40 Issue 4 Pages T83-T86
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA simple and reproducible method for the determination of clospipramine in plasma by HPLC has been developed. Sample preparation and procedures for HPLC were as follows; 1-heptane containing 1.5% isopentyl alcohol (n-HIAA) was added to alkalized plasma using 5-[3-(2-oxo-1, 2, 3, 5, 6, 7, 8, 8a-octahydroimidazo [1, 2-a] pyridine-3-spiro-4'-piperidino)propyl]-10, 11-dihydro-5H-dibenzo[b, f] azapine) (Y-15364) as an internal standard. After shaking and centrifugation of the sample, the aqueous phase was frozen in a dry ice-2-propanol mixture. The organic phase was transferred to another tube. Drugs were extracted with dilute hydrochloric acid. This acidic solution was frozen in a dry ice-2-propanol mixture; and the organic phase was discarded. The acidic solution was made alkaline, then extracted with n-HIAA, and again frozen in a dry ice-2-propanol mixture. The organic phase was transferred to another tube and dried under a stream of N2. The residue was dissolved in 30μl of 38% acetonitrile solution. Twentyfive microliters of the solution were injected into the chromatograph which was equipped with a system Model 510, U6K injector, μ Bondasphere 5 phenyl-100Å column (3.9mm×15cm), and Model 481 UV detector setting at 254nm (Nihon Waters Ltd.). The flow rate of the mobile phase {38% acetonitrile containing 10mM dibutylamine phosphate (pH 3.0)} was 0.7ml/min. The retention times for Y-15364 and clospipramine were 6.0 and 8.5min, respectively. The limit of detection was 1.0ng/ml for clospipramine in plasma. Within-run reproducibility datum for 50ng/ml is 3.5% (n=7). The result of the measurement of the clospipramine concentration in plasma after a single oral administration to schizophrenic patients, indicates that the proposed method would be applicable in clinical treatment of antipsychcotic drugs.View full abstractDownload PDF (388K) -
Shigeki OOBA1991 Volume 40 Issue 4 Pages T87-T90
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn automatic titrator which allows the titration under the condition of a slow exchange rate was trially manufactured and tested using zirconium phoshate. This instrument consists of an ion meter, autopiston burette, digital multimeter and a personal computer. The results of each titration volume, pH and titration curve were recorded using the auto-matic titrator. The measurement time, of each titration volume and end point condition were variable in order to accommodate the user's request. In this study, standard measurement times (smt) for each titration volume were 1, 2 and 4h. When the smt did not satisfy the condition for an end point in each series of titration experiment, these smt were extended within the maximum measurement termination times (mmtt). These mmtt were set at 4h for smt of 1, 2 and 6h for smt of 4h, respectively. The titration curve for zirconium phosphate using sodium hydroxyde indicates two steps. At smt of 1h, the system did not reach equilibrium, which can be detected by two peaks appearing at the second equivalence point. It is possible to identify the second equivalence point by careful analysis of the titration record. The results are satisfactory for the smt of 1, 2 and 4h, though the curve of smt at 1h shows little difference from others, except for a more complicated structure at the second equivalence point.View full abstractDownload PDF (513K) -
Tsutomu MATSUO, Akihiko MUROMATSU, Yasutaka SAHARA1991 Volume 40 Issue 4 Pages T91-T95
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA simple and inexpensive optical fiber photosensor (OPS) has been developed. A halogen bulb and light intensity sensor were used as a light source and a detector, respectively. The optical fibers serve to conduct the light from the bulb to the test solution and collect the transmitted light. Since the detector cell is small and isolated, it is usuable for in remote sensing and free from any hazardous environment. The sensitivity is comparable to the photosensor previously reported. The optical fiber photosensor was applied to the acid-base, chelate and precipitation titrations.View full abstractDownload PDF (534K) -
Haruo TUJI, Yuzo TAMARI, Sayaka KATAGIRI, Kenji YAMAZAKI, Yuzuru KUSAK ...1991 Volume 40 Issue 4 Pages T97-T100
Published: April 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor the determination of arsenic(III), arsine was first generated from the sample solution at pH 9 with tetrahydroborate, and then it was introduced into a heated quartz glass cell along with argon; and finally the atomic absorption of arsenic was measured. In addition, the total arsenic was determined under acidic condition (5% hydrochloric acid solution) in the same manner. The arsenic(V) was determined by subtracting the value of arsenic(III) from that of total arsenic. This method was applied for ground and river water samples. Detection levels of 2.6-8.0 ppb of arsenic(V) were detected, whereas arsenic(III) was not detected.View full abstractDownload PDF (546K)
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