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Volume 34, Issue 8
Displaying 1-16 of 16 articles from this issue
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Hiroshi NAKAMURA1985 Volume 34 Issue 8 Pages 423-463
Published: August 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESS -
Second derivative fluorometric methodYuichi TAKAYAMA, Shiro GOHDA, Kiyotoshi MORISHIGE, Tsunenobu SHIGEMATS ...1985 Volume 34 Issue 8 Pages 465-471
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDysprosium-EDTA complexed with sulfosalicylic acid (SSA) was synthesized, and the fluorescence properties and radiation process of the ternary complex have been studied. The Dy-EDTA-SSA ternary complex shows distinct fluorescence (Ex 325 nm, Em 576 nm, Φf 0.049, F.S.I. 2.2×10-3 μm, τf 2.6 ms) which is attributed to radiative transition from 4F9/2 level to 6H13/2 level of centered Dy(III). This communication reported the optimum conditions for the fluorometric determination of Dy(III), and 2nd derivative fluorometric method was utilized for the analysis of trace amount of Dy(III) in xenotime and monazite minerals. The procedure for the determination of Dy(III) in minerals was established as follows: The rare earth mineral samples (xenotime and monazite) treated with hot conc. H2SO4 and twice precipitated with 0.5 mol dm-3 oxalic acid (pH was adjusted to 2.02.2). Then the precipitates was filtered and ignited to give the rare earth oxide. Five hundred milligrams of the oxide was dissolved in conc. HCl and diluted with water in order to obtain the solution containing 50 μg cm-3 rare earth oxide. In the case of monazite sample, an extraction procedure with di- (2-ethylhexyl) phosphine oxide/ cyclohexane solution is used for the separation of Dy(III) from light rare earth {La(III), Ce(III), Pr(III), Nd(III), and so on}. To aliquot of the solution (0.21.5 cm3) containing less than 2.0μg as rare earth oxide, were added 1.0 cm3 of 2.5×10-3 mol dm-3 EDTA solution, 1.0 cm3 of 2.5×10-2 mol dm-3 SSA solution and 10 cm3 of 1.0 mol dm-3 diethylamine-hydrochloric acid buffer solution. The pH of the solution was adjusted to pH 11.9±0.1, and the solution was diluted to 25 cm3 with water. The 2nd derivative fluorescence intensity [Ex: 325 nm, Em: 576 nm] was measured. Several rare earth mineral samples were analyzed. Xenotime contained 5.08% of Dy2O3 and monazite contained 1.83% of Dy2O3.View full abstractDownload PDF (1154K) -
Jun'ichi ITO, Hideki KAWASHIMA, Katsunori ENDO, Michio MAEDA, Tsutomu ...1985 Volume 34 Issue 8 Pages 472-477
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA soil sample of 5 to 10 g was subjected to the first heavy liquid separation using 80 ml of tribromomethane (ρ=2.65 g cm-3) and a centrifuge in order to concentrate silicon carbide in the sediment. Decomposable silicates and others in the sediment were removed by hydrofluoric acid treatment, digestion in other acids and centrifuging. The resulted residue was subjected to the second separation in a heavy liquid separation tube using 10 ml of a Clerici solution (ρ=3.62 g cm-3) to isolate silicon carbide as float. The float filtered on a filter paper and a membrane filter was ignited. The silicon carbide thus obtained was weighed and examined for the structure type, interferences, particle size etc. by X-ray diffraction and fluorescence analyses and microscopic observation. Such information is also helpful especially for the discussion of the origin of a soil sample. The lower limit of the determination is about 0.02%. Interferences for the identification, recovery, and examples of determination arc also given.View full abstractDownload PDF (1205K) -
Masanobu HABIRO, Yoshinori SUGITANI, Kozo NAGASHIMA, Kenji KATO, Masuo ...1985 Volume 34 Issue 8 Pages 478-482
Published: August 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA simple and rapid method for photoacoustic determination of water in nitrogen has been developed by the use of a resonance photoacoustic cell. The cell is a double tube type suitable for measurements under flow conditions. The change of the resonance frequency resulting from fluctuation of temperature in the cell was compensated by adjusting the chopping frequency so that the maximum photoacoustic intensity was obtained. Sample gases containing various concentrations of water under the total pressure of 1 atm were generated by the diffusion method for lower concentrations range. The laboratory made apparatus which utilizes the permeation of water into teflon tube was used for higher concentration regions. Plots of the photoacoustic intensity versus concentrations showed a linear relationship between 25 and 1725 ppm water. No saturation was observed even at 1725 ppm. The detection limit (at S/N=2) was 2.5 ppm.View full abstractDownload PDF (738K) -
Fumio IINUMA, Masayoshi TABARA, Kazuko YASHIRO, Mitsuo WATANABE1985 Volume 34 Issue 8 Pages 483-486
Published: August 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSThe fluorescence of kynurenic acid in aqueous media was found to be greatly enhanced by the addition of 100 mM zinc(II) acetate. This finding was successfully applied to improve the assay procedure of kynurenic acid in urine. The procedure is as follows. To 1 ml of human urine were added 2 ml of distilled water and 1 ml of 0.1 M hydrochloric acid, and the solution was passed through a column of Dowex 50W-X12 (H+ form, 200400 mesh, 3 cm×0.3 cm i. d.). The column was washed successively with 2 ml of 0.1 M hydrochloric acid, 2 ml of 0.2 M hydrochloric acid, 3 ml of 0.5 M hydrochloric acid, and 0.5 ml of distilled water. Kynurenic acid was eluted with 9 ml of distilled water.To 2 ml of this effluent was added 1 ml of 0.3 M zinc (II) acetate reagent. The fluorescence intensity of the solution excited at 344 nm was measured at 398 nm. The calibration curve for kynurenic acid showed a linear relation in the range of 150 pmol to 4.5 nmol. The relative standard deviation at 4.5 nmol was 1.36% (n=6). In this procedure, the recovery of kynurenic acid in the five samples of urine was found to be 97.2 ± 11.6% (n=5). Kynurenic acid contents in urine of healthy adults which were collected for 24 h were 6.929.22 μmol/d (male, 39 years old, n=5) and 7.5513.76 μmol/d (male, 31 years old, n=5).View full abstractDownload PDF (641K) -
Toshio ISHIZUKA, Yoshinori UWAMINO, Akira TSUGE1985 Volume 34 Issue 8 Pages 487-491
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSInductively coupled plasma emission spectrometry(ICPES) was used to determine impurities (Al, Ca, Fe, Hf, Mg, Mn, Na, Si, and Ti) in zirconium oxide powder samples. Sample solutions were obtained by acid decomposition with hydrofluoric or sulfuric acid in a Teflon pressure vessel. In the hydrofluoric acid decomposition, 0.5 g of zirconium oxide was dissolved with 2.5 ml of (1+1) hydrofluoric acid and 2.5 ml of hydrochloric acid at 150°C for 5 h. After the addition of 20 ml of 4% boric acid for masking fluoride ion, sample solution was diluted to 100 ml with distilled water, followed by ICPES determination. In the sulfuric acid decomposition, 0.5 g of zirconium oxide was dissolved with 5 ml of (1+1) sulfuric acid at 230°C for 16 h, and diluted to 100 ml with distilled water. The zirconium matrix in the two sample solutions appreciably reduced the emission intensities of the elements and increased the background levels. Thus, it was necessary to add the matrix component to standard solutions to get compositions similar to those of sample solutions. Masking of fluoride ions with boric acid seems inadequate to prevent the dissolution of the quartz torch, and the hydrofluoric acid decomposition method gave a higher background intensity at Si I 251.61 nm, a higher detection limit of Si, and a larger scattering in the measured values of Si contents. For other elements except Si, the method of sample decomposition had little effect on both the detection limit and the analytical values of the elements.View full abstractDownload PDF (970K) -
Sadao MORI, Masatoshi KATO, Masami SUZUKI1985 Volume 34 Issue 8 Pages 492-496
Published: August 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSDiol bonded porous glass packing materials of average particle diameter 5 or 10μm and of pore sizes 170 Å and 500 Å were packed into a 7.2 mm i.d.×25 cm length column by a slurry packing procedure. Slurry solvents were the mixtures of methanol and ethylene glycol which had appropriate viscosity for packing materials. Packing solvent was n-heptane which was immissible with the slurry solvent. A 5-g portion of porous glass was mixed with the slurry solvent and packed into a column in 5 min under the constant flow by regulating the pressure of the packing solvent up to 500 kg/cm2 with a pneumatic pump. Viscosity of the slurry solvent should be controlled to suit particle sizes and pore diameters of the packing materials by changing the composition of methanol and ethylene glycol. Efficiency of the column thus obtained was 12000 theoretical plates per 25 cm by using ethylene glycol as a test sample and water as the mobile phase. Exclusion limit of the packing materials of 170 Å pore size was about 200000 as pullulan and that of 500 Å pore size was 1000000. These columns can be used for aqueous size exclusion chromatography.View full abstractDownload PDF (736K) -
Kunihiro WATANABE, Izuo AOKI1985 Volume 34 Issue 8 Pages 497-503
Published: August 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSIn the previous studies on the determination of beryllium with salicylidene-2-aminophenol(SAPH), it has been shown that the Schiff base reacts with the metal ion to form Be-SAPH complex. In the present paper the authors have investigated the composition of Be-Schiff base complex in the presence of large amount of amine, so that SAPH reacts with amines to form another respective Schiff bases. The optimum condition were studied for the fluorometric determination of beryllium with salicylaldehyde and some of its derivatives and bissalicylidene-ethylenediamine in place of SAPH. The optimum pH range for formation of the Be-Schiff base complexes, which depends on the kind of amine, was from 8 to 12. Effects of 19 amines discussed : N, N-dimethyl-1, 3-propanediamine was superior to other amines. 2-Hydroxy-5-methylbenzaldehyde combined with N, N-dimethyl-1, 3-propanediamine was better than other couples as a reagent. The recommended procedure for the fluorometric determination of beryllium is as follows : Take a sample solution containing less than 4 μg of beryllium. Add 5 ml of a mixture (pH 10) of N, N-dimethyl-1, 3-propanediamine (10%) and hydrochloric acid. Then add 1 ml of 0.01% bis (5-methylsalicylidene) ethylenediamine methanol solution. Dilute to 25 ml with water. The fluorescence intensity at 455 nm is measured at excitation wavelength of 350 nm, in which a quinine sulfate solution is used as a reference. Accurate determination is possible in the concentration range of beryllium from 0.002 μg to 4 μg.View full abstractDownload PDF (1013K) -
Han-guo HUANG, Xiao-an WANG1985 Volume 34 Issue 8 Pages 504-507
Published: August 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSThe separation of rare earth metal ions by high voltage paper electrophoresis(HVPE) using citric acid as electrolyte, and determination of samarium and europium by means of extraction fluorometry with 2-thenoyltrifluoroacetone (TTA) and 1, 10-phenanthroline (phen) have been investigated. It has been found that migration distance of rare earth metal ions shortened with increasing atomic number and decreasing ionic radius of tervalent rare earth ions. Light rare earth ions, La3+-Ce3+-Pr3+-Nd3+-Sm3+(Eu3+), could be separated from each other and the separation of these ions from heavy rare earths as well as from Fe3+-Sc3+-Y3+ could also be achieved by using following conditions : electrolyte, 0.05 M citric acid solution (pH 2.22) ; voltage applied, 3000 V; separation times, 25 min. The recovery of the samarium and europium is 94.0% and 97.8%, respectively, in the range of 20800 ng/ 10 ml of these ions using TTA-phen benzene extraction fluorometry after HVPE. In this way, mixtures of rare earth oxides are analyzed, 0.023μg of Eu2O3 and 0.026μg of Sm2O3 being precisely determined.View full abstractDownload PDF (733K) -
Hisakazu NOZOYE, Kazuo SOMENO1985 Volume 34 Issue 8 Pages 508-509
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSHigh-purity silane is a raw material for semiconductor devices or solar cells. The quantitative analysis of low levels of phosphine is practically very important but there are few published reports on the gas chromatographic analysis of phosphine in silane. A Shimadzu GC-7A gas chromatograph equipped with a flame photometric detector and a stainless column filled with Porapak Q (80100 mesh) was used. The column temperature was 100°C and the flow rate of helium carrier gas was 60 ml/min. The volume of the sample loop was 2.8 ml. The pre-cut method was used since the difference in the retention times of phosphine and silane was enough to separate them with a stainless steel column (5 m×3 mm i. d.). Low levels of phosphine ranging from 10 ppm to 0.5 ppb could be quantitatively analyzed by the present method.View full abstractDownload PDF (322K) -
Kunihiro WATANABE, Kakuji TAKAHASHI1985 Volume 34 Issue 8 Pages 509-512
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIt has been reported that selenium and tellurium react with bismuthiol II to form 1 : 4 complexes(Se or Te : reagent). In this work the composition of the complexes precipitated from an aqueous phase was also confirmed to be 1 : 4 by elementary analysis. However, it was revealed that the complexes were mixtures of Se(II)- and/or Te(II)-bismuthiol II, and disulfide of the reagent by vapor pressure osmometry. Selenium (IV) and Tellurium(IV) oxidize a part of the reagent to disulfide and are themselves reduced to Se(II) and Te(II), followed by combining with the reagent to from the Se- and Te-bismuthiol II complexes. This reaction is quantitative and the disulfide contained in the precipitate was confirmed by IR spectra. Once large amounts of the precipitates are dissolved in benzene and chloroform, they soon reprecipitate from the organic phase. The precipitates were confirmed to be 2 : 2 complexes by elementary analysis, mass spectra, and gel permeation chromatography.View full abstractDownload PDF (691K) -
Toshio YAO, Yoshihiro MATSUMOTO, Tamotsu WASA1985 Volume 34 Issue 8 Pages 513-515
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA flow injection system for enzymatic determination of ethanol in serums is described. A phosphate buffer (0.1 M, pH 8.0) containing 1 mM potassium hexacyanoferrate(II) served as the carrier solution and was pumped at a constant flow rate of 1.4 ml min-1. The system includes an amperometric peroxidase electrode to measure hexacyanoferrate(III) converted from hexacyanoferrate(II) by hydrogen peroxide, which is generated by injecting 10-μl sample into an immobilized alcohol oxidase reactor. The peroxidase electrode operates at 0.0V vs. Ag/AgCl. The peak current was linearly proportional to the ethanol concentration in the range of 0.0210mM; 120140 samples per h could be processed with satisfactory precision(12% R.S.D.).View full abstractDownload PDF (616K) -
Akira MIYAZAKI, Akira KIMURA, Hiroaki TAO, Kenji BANSHO1985 Volume 34 Issue 8 Pages 515-518
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSFor the rapid and sensitive determination of metals in water by inductively coupled plasma emission spectrometry (ICP-ES), a combination of simple solvent extraction with a modified volumetric flask and introduction of the extract to the ICP torch by ultrasonic nebulization was investigated. Sample solution (260 ml), ammonium pyrrolidinedithiocarbamate (APDC) solution, hexamethyleneammonium hexamethlenedithiocarbamate (HMAHMDC) methanolic solution, acetate buffer(pH 4.2), and 8 ml of diisobutylketone(DIBK) were stirred vigorously in the extraction vessel for 7 min by a magnetic stirrer. The extract was introduced into the ultrasonic nebulizer by the displacement bottle method and analyzed by ICP-ES. Detection limits for Cd, Co, Cu, Fe, Mo, Ni, Pb, Zn, and V of the method were consistently lower than those by a pneumatic nebulizer. Metal blank was lower (<0.005μg) than that of the separatory funnel method. The proposed method was applied to the analysis of NBS SRM 1643a, metal plating plant waste waters, and coastal seawaters.View full abstractDownload PDF (734K) -
Hiroshi MIKASA, Shoji MOTOMIZU, Kyoji TÔEI1985 Volume 34 Issue 8 Pages 518-521
Published: August 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSFlow injection analysis(FIA) was examined for the fluorometric determination of ammonia in river water. Ammonia reacted with ο-phthalaldehyde(OPA) in the presence of 2-mercaptoethanol(ME) to form a fluorescent substance at pH 9.5. The reagent solution containing 10-2 M OPA and 10-3 M ME and the carrier fluid(distilled water) were propelled by a double plunger pump at a rate of 1.2 ml/min. The 40μl sample solution, injected into the carrier stream, was mixed with the reagent solution in a Teflon tubing (3 m, 0.5 mm i.d.) and led to a flow cell(18 μl). Fluorescence excited at λex=350 nm was measured at λem=486 nm. Ions present commonly in river waters did not interfere with the determination of ammonia. An anion exchange column installed just behind a sample injection valve in the flow system was effective in eliminating interferences with amino acids. Using the proposed FIA system, trace amounts of ammonia(3150 ppb as nitrogen) in river water were determined in the rate of 40 samples per h.View full abstractDownload PDF (593K) -
Kamihiko ITSUKI, Hiroaki YAGASAKI, Hiroshi FUJINUMA1985 Volume 34 Issue 8 Pages T109-T112
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAtomic absorption spectrometry using a graphite furnace for the determination of minute amounts of indium was developed from our previous method for tin, antimony, arsenic, and tellurium. For the atomization, nitric acid solution is preferable and they should be free from hydrochloric acid and sulfuric acid. Interferences induced potentially by aluminum, chromium, antimony, tin, and tartaric acid could be prevented by an addition of 2000 ppm of lanthanum as nitrate. Less than 20μg of indium was coprecipitated with 20 mg lanthanum and 1 mg iron from an aqueous ammonia solution and was separated from unexpected interfering materials. The method was applied to the determination of indium in zinc concentrates.View full abstractDownload PDF (492K) -
Motonori ETOH, Kyohji NARIMATSU, Sadao NAGAI1985 Volume 34 Issue 8 Pages T113-T115
Published: August 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA titrimetric method for the determination of palladium in carbon based palladium catalyst was examined. The sample was ignited at 650°C and then decomposed with aqua regia. Five ml of sulfuric acid was added and brought to boiling until very dense white fumes of sulfuric acid were evolved. After cooling, it was diluted to 150 ml with distilled water, then titrated potentiometrically with a standard potassium iodide solution. The presence of chloride ion or silver as matrix component affected the determination of palladium. The chloride ion could be eliminated by evolving the white fume of sulfuric acid, and the effect of silver was negligible because silver concentration in sample solution was less than 20 ng/ml. This method was applied to the analysis of carbon based palladium catalyst(Pd : 0.5%, 5%). The results were in good agreement with the values obtained by a gravimetric method. The relative standard deviation was less than 0.2%.View full abstractDownload PDF (425K)
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