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Volume 34, Issue 9
Displaying 1-16 of 16 articles from this issue
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Masanori OWARI, Makoto GOTO, Naoto OIWA, Akihiro FUKUDA, Giichi MUTO, ...1985 Volume 34 Issue 9 Pages 523-528
Published: September 05, 1985
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSIn order to extract chemical character of coal fly ash particulates, one by one X-ray micro analysis of fly ash particulates and statistical data processing were performed. Domestic, foreign and NBS 1633a coal fly ash were used as samples. For each fly ash, 150 spherical particulates of which diameters were in the range 0.520 μm were selected, and Kα X-ray intensities of sodium, magnesium, aluminum, silicon, phosphorous, sulfur, potassium, calcium, titanium, vanadium, and iron were measured. No clear correlation was found between compositional values or between compositional values and particulate diameters. Pattern recognition technique based on distances on eleven-dimensional space represented by compositional values was applied to classify compositional distribution patterns of particulates. As a result, some types of particulate groups each of which had the characteristic compositional pattern were found. The largest group had the compositional pattern similar to that of the whole average. Other groups were characterized by the compositional values of calcium or iron. Particulates with very distinctive compositional patterns were also found. Analyses on density-separated fractions revealed that most of the particulates with the density less than 2.8 g/cm3 had similar compositional patterns with each other, irrespective of the density. Such results indicated that many particulates had interior vacancies.View full abstractDownload PDF (907K) -
Seiichiro HIGUCHI, Zegen ZHENG, Shigeyuki TANAKA1985 Volume 34 Issue 9 Pages 529-533
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe microanalytical examinations were made by the preresonance Raman spectrometry for 2-nitrofluorene, 1-nitropyrene, 4-nitrobiphenyl, 5-nitroacenaphthene, and 4, 4'-dinitrobiphenyl. They are found in airborne particles sampled at highways or in the waste gases of coals as components soluble in organic solvents. These samples have UV absorption bands in the wavelength region from about 300 to 400 nm. The wavelength of the excitation laser line is 488.0 nm. The resonance enhancement of the intensities of Raman bands was observed by the laser excitation at 488.0 nm. It was shown that the fluorescence background became markedly lower when the sample solutions were exposed to laser irradiation, at least, in this particular case using CCl4 as a solvent. The excellent selectivity of the present method was demonstrated by comparing the spectra of each compound with those of mixed samples. The detection limits determined from the NO2 symmetric stretching band and the bands inherent in each sample, ranged from 10-6 M to 10-8 M. The analytical curves were linear over a wide concentration range. It was concluded that the Raman spectrometry is one of the very useful methods for identification and determination of the carcinogenic nitrocompounds in environmental samples.View full abstractDownload PDF (707K) -
Yoshihito SUZUKI, Kazue TANI, Kuniko MIYAZAWA1985 Volume 34 Issue 9 Pages 534-538
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSEffects of mobile phase composition and column temperature on retention behavior were investigated for 2, 4-dinitrophenylhydrazones (2, 4-DNPH) derived from aromatic monosubstituted aldehydes. The chromatographic separation of these derivatives was attempted by the use of ODS column with binary mixture of methanol and water as a mobile phase. The separation of various 2, 4-DNPH's was unsatisfactory at column temperature 40°C with mobile phase composition from 70% to 90% methanol. However, separation selectivity was improved by elevating the column temperature. The plots of ln k' versus 1/T were linear within the temperature range studied. From the linear plots, the values of enthalpy changes ΔH° and (ΔS°/R+lnVs/Vm) were determined. Para isomers were found to be eluted faster than ortho isomers. This was attributed to the larger entropic contribution than the enthalpic one.View full abstractDownload PDF (671K) -
Shigehiko YAMAGUCHI, Shinichi YOKOYAMA1985 Volume 34 Issue 9 Pages 539-543
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA compositional analysis method of styrene-acrylate-methacrylate terpolymers by pyrolysis gas chromatography (PGC) is described. In the PGC analysis of the terpolymers, it is necessary to take the boundary effect into account satisfactorily. Styrene-ethyl acrylate-ethyl methacrylate terpolymers were used as model compounds. Pyrolysis was performed at 590°C using a Curie point pyrolyzer. Acrylate/methacrylate ratio of the terpolymers could not be determined with the previously proposed method {This journal, 33, 153 (1984)}, because of much difference in thermal degradation behavior between methacrylate-acrylate and styrene-acrylate bonds. It was found that correlation factor between acrylate/methacrylate ratio in the terpolymers and in their pyrolytic products could be estimated from three dimension plots of acrylate monomer/dimer ratio-styrene/methacrylate ratio-correlation factor, which was plotted using the results of PGC for 18 samples of styrene-ethyl acrylate-ethyl methacrylate terpolymer prepared in our laboratory. Stylene/methacrylate ratio in the terpolymers could be determined using similar plots. The compositions of stylene-ethyl acrylate-butyl methacrylate terpolymers were successfully determined by the proposed method.View full abstractDownload PDF (706K) -
Kazuhiko TSUKADA, Takashi IKEGAMI, Hidetoshi ARAKAWA, Masako MAEDA, Ak ...1985 Volume 34 Issue 9 Pages 544-548
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA sensitive fluorescent enzyme immunoassay for the determination of thyroxine(T4) in dried blood samples spotted onto filter paper and in serum has been developed. Thyroxine was conjugated to glucose oxidase by glutaldehyde method. Separation of free and bound fractions after immune reaction, was done by using polystyrene tubes coated with anti-T4-antibody on anti-rabbit-antibody (second antibody). The enzyme activity was measured by fluorometric reaction using p-hydroxyphenyl acetic acid and horseradish peroxidase after incubation with glucose. The detection limit of the present method was 5 pg/assay tube for T4. The intra- and interassay relative standard deviations were 4.011.2 % and 5.112.3%, respectively. The correlation between proposed method and radioimmunoassay was good (r=0.88 and 0.90, n=100).View full abstractDownload PDF (635K) -
Suwaru HOSHI, Sadanobu INOUE, Mutsuya MATSUBARA1985 Volume 34 Issue 9 Pages 549-553
Published: September 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSIn the presence of some masking agents, the ion-pair of zinc (II)-1, 10-phenanthroline (phen) complex cation with tetraiodofluorescein (TIF) can be extracted selectively into chloroform from alkaline solution(pH 7.5 10.5). The extracted complex has a composition of [Zn(II)-(phen)2](TIF). This extraction method was applied to the spectrophotometric determination of zinc. The recommended procedure is as follows. To a solution containing up to 2.0μg of zinc in a separatory funnel, 1 ml of 0.025 M phen, 5 ml of 0.1 M borax buffer(pH 9.3), and 2 ml of 1.25×10-3 M TIF are added and the mixture is made up to 25 ml with water. After 5 min, the solution is shaken with 5 ml of chloroform for 7 min. After two phases are separated with a centrifuge, the absorbance of organic phase is measured at 549 nm against the reagent blank. Beer's law holds up to 0.22.0 μg of zinc and its apparent molar absorptivity at 549 nm is 1.15×105 dm3 mol-1 cm-1. Pretreatment method was also investigated by using a strong base anion exchanger for lower tolerant metals {Ni(II), Mn(II), and Cu(II)}.View full abstractDownload PDF (465K) -
Kazuo IMAEDA, Keiko OHSAWA, Katsumi UCHIYAMA, Akihiro MUTOH1985 Volume 34 Issue 9 Pages 554-558
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSUltra weak chemiluminescence occurs when a material is degraded. Degradation of macrogol 4000 was evaluated by measuring the ultra weak chemiluminescence. Intensity of ultra weak chemiluminescence from degraded macrogol 4000 by UV irradiation was compared with the oxygen content of the same material determined by direct oxygen determination method. An apparatus made for measuring ultra weak chemiluminescence consists of a photomultiplier tube R585 (Hamamatsu Photonics, Co., Ltd., Japan), a sample holder which is incorporated in a black box, a thermo-controller, and a photon counter C1230 (Hamamatsu Photonics, Co., Ltd., Japan). Macrogol 4000 was irradiated for 048 h by UV rays (maximum radiation band: 254 nm) at an intensity of 5μW/cm2. Intensity of ultra weak chemiluminescence reached a maximum after 3h of UV irradiations. Over 3h of UV irradiation, the intensity of chemiluminescence decreased. Oxygen content of macrogol 4000 showed the maximum (41.5%) at 5 h of UV irradiation. The value was about 4.8% higher than the theoretical oxygen content of macrogol 4000 (36.7%). The pH value of an aqueous solution of macrogol 4000 (1g/100 ml) the decreased according to UV irradiation time. The greatest decrease in the pH was observed at 57 h of UV irradiation. The IR spectra of macrogol 4000 (for 648 h of UV irradiation) showed a weak absorption band at about 1700 cm-1 corresponding to a carbonyl group. From these results it was suggested that the dissolved oxygen in the macrogol 4000 gave peroxyradical resulting in a high energy state aldehyde or ketone group for 03h of UV irradiation, so the intensity of ultra weak chemiluminescence increased. For 35h UV irradiation, macrogol 4000 incorporated atmospheric oxygen as the carbonyl group was oxidized to give carbonic acid or peroxy acid. After 5 h UV irradiation, the ether bonds of macrogol were cleaved to give volatile materials such as formaldehyde, formic acid, acetoaldehyde, and acetic acid. As these volatile acids or aldehydes vaporized in the air, oxygen content of macrogol decreased to the initial level. A combination of the measurement of ultra weak chemiluminescence and the direct oxygen determination would make a reliable and accurate evaluation method for degradation of materials.View full abstractDownload PDF (790K) -
Taichi SATO, Hiroshi WATANABE, Hiroshi NAKAMURA1985 Volume 34 Issue 9 Pages 559-563
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe extraction of lactic, tartaric, succinic, and citric acids from aqueous solutions by trioctylamine (TOA, R3N) was investigated under various conditions. As a result, it was found that the concentration of acid in the organic phase increases with increasing aqueous acid concentration and this tendency is little influenced at different TOA concentrations. The log-log plots of distribution ratio vs. [TOA] revealed the following power dependence: 0.51 for lactic acid, 12 for tartaric and succinic acids, and 13 for citric acid. Hence the extraction of organic acids by TOA is expressed by the equilibrium equation HnA(ap)+ mR3N(org)_??_(R3N)mHnA(org) where n and m=1 for lactic acid, n=2 and m=12 for tartaric and succinic acids, and n=3 and m=13 for citric acid. The formation of the organic species is also supported by infrared spectral results. Moreover the temperature-dependence of distribution ratio indicates that the extraction of organic acids decreases with increasing temperature.View full abstractDownload PDF (732K) -
Hiroshi NISHIDA1985 Volume 34 Issue 9 Pages 564-567
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSVanadium(V) formed a water soluble complex with 8-quinolinol (HL) in the presence of Triton X-100 at pH 3.2, showing two absorption maxima at 410 nm and 530 nm. Then the black-red color development was applied to the spectrophotometric determination of vanadium(V). Recommended procedure is as follows: To less than 400μg of vanadium(V) in an acidic medium, add 5 cm3 of Triton X-100 solution (0.12 g cm-3) and 2.0 cm3 of 8-quinolinol solution (9.6×10-2 mol dm-3). Adjust pH to 3.2 with sodium acetate solution (1 and 0.2 mol dm-3) and dilute to 20 cm3 with water. Heat for 10 min in a water bath at 60°C, cool to room temperature with water and dilute to 25.0cm3 with water. Measure the absorbance at 530 nm against the reagent blank. Beer's law was valid over the range of 0.416 ppm of vanadium(V). The molar absorptivity at 530 nm was 2.9×103 dm3 mol-1 cm-1. Up to 10 mg of Ca(II), Mg(II), Mn(II), Cd(II), Pb(II), 5 mg of Ni(II), Co(II), Zn(II), Al (III), 2 mg of Mo(VI), 0.5 mg of Cr(III), 0.2 mg of W(VI), and 0.1 mg of Ti(IV) did not interfere. Interference from less than 50 mg of Fe(III) and Cu(II) was removed as precipitate of their 8-quinolinolates from its alkaline solution in the range of pH 1011. It was considered that the complex showing the absorption maximum at 530 nm was VO(OH)L2.View full abstractDownload PDF (513K) -
Kazuhide UCHIDA, Masako TOMODA, Shinichi SAITO1985 Volume 34 Issue 9 Pages 568-572
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSFlow injection analysis is proposed for the rapid and simple determination of calcium in natural and tap waters with spectrophotometric detection. The method is based on the color change reaction between calcium in the sample and indicator at pH 13. The change in the absorbance of Hydroxynaphthol Blue (HNB) owing to the complex formation of HNB with calcium is measured spectrophotometrically at 455 nm, for calcium in the sample. No masking reagent for magnesium is required because magnesium hydroxide forms at high pH. The flow injection system was investigated to obtain the optimum conditions for the following: mixing coil length, reaction coil length, flow rate, pH and wavelength. The effects when metals were added to the calcium standard solution were examined. Barium, zinc, and aluminium did not interfere at all. Magnesium, strontium, and iron did not interfere in amounts up to the amount of calcium present. Nickel, copper, and manganese gave negative errors, and cadmium gave a positive one. A linear relationship was observed between concentration of calcium (from 1.2 to 3.9 mg dm-3) and absorbance. This method allows the analysis of ca. 40 samples per h. The relative standard deviation was 1.12% (n=15). The results for analysis of natural and tap waters agreed well with those obtained by standard EDTA titration with NN as indicator. For a single analysis the sample volume injected was as little as 50 mm3; no complicated operation is required. When the pH range of sample is from weak acid to strong base, no buffer solution is required.View full abstractDownload PDF (760K) -
Kunio NAKANO, Shigeru ICHISUGI1985 Volume 34 Issue 9 Pages 573-575
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn this paper direct determination of silver collected on ion-exchange filter paper was studied. 50 ml of sample solution of which pH was adjusted to 3.3 with hydrochloric acid was passed through a sheet of ion-exchange filter paper, and after the filter paper was dried, it was punched with a 2.5 mm puncher. The small tablet was put onto a tungsten atomizing furnace and electrothermally heated. The calibration curve was linear at Ag+ concentrations below 0.3 ng/ml, and 1% absorption sensitivity was 1.2×10-3 ng/ml. Coexsisting 104-fold Na+, 103-fold Cu2+, and 103-fold Pb2+ did not affect the absorbance of Ag. Detection limit of this method is considered to lower by increasing the volume of sample solution.View full abstractDownload PDF (385K) -
Yoshihito SUZUKI, Hitoshi KOIZUMI, Naoto HIRANO1985 Volume 34 Issue 9 Pages 575-579
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSGas chromatographic separation of isomers of mono substituted phenols as their alkyl ether derivatives was studied on liquid crystal stationary phase. Three Schiff's base type liquid crystals such as 4-(p-methylbenzyloxy)benziliden-4'-n-alkylaniline (alkyl; ethyl→MBBE, 1-butyl→MBBB, 1-hexyl→MBBH) were prepared as stationary phases. The temperature ranges of nematic mesophase for MBBE, MBBB, and MBBH were 122140°C, 132147°C, and 132140°C, respectively. A mixture of alkyl ether derivatives from mono-substituted phenols was chromatographed on a column (3 mmφ×2 m or 3 m, stainless steel) packed with 10% liquid crystal at the temperature of nematic mesophase. p-Substituted ether derivatives provided larger retention volume and better selectivity than other isomers. It was found that phenols tested could be quantitatively converted into their ethers with 1-propyl bromide.View full abstractDownload PDF (558K) -
Tadashi IWACHIDO, Masanao TAJIRI, Kyoji TÔEI1985 Volume 34 Issue 9 Pages 579-581
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn extraction-spectrophotometric method for the determination of potassium by means of a new reagent, 4-[(4-(phenylamino)phenyl)azo]-2, 5-dichlorobenzenesulfonic acid (TOOCl2) was proposed. The complexes of potassium ions with dibenzo-18-crown-6 (DB18C6) associate with TOOCl2 anions to give colored ion pairs which can be extracted into benzene. The ion pairs in benzene exhibit a maximum absorption at 430 nm with an apparent molar absorption coefficient of 9300 dm3 mol-1 cm-1. Potassium in river water was determined as follows: To a 50-cm3 vessel with a stopper, 5 cm3 of an aqueous TOOCl2 solution (0.02 mol dm-3), 5 cm3 of an aqueous Li2(EDTA) (0.001 mol dm-3) solution, and 10 cm3 of a water sample were transferred. The resulted solution was shaken with 20 cm3 of a benzene solution of DB18C6 (0.01 mol dm-3) for 30 min at 20°C. After the mixture was allowed to stand for 30 min, the absorbance of the benzene phase was measured at 430 nm against a reagent blank. Interferences from calcium (II) and magnesium (II) were avoided by complexing with EDTA. Sodium ions up to 8 ppm gave virtually no interference. Potassium concentrations determined by means of the proposed method agreed closely with those of atomic absorption spectrophotometry.View full abstractDownload PDF (436K) -
Osamu NARA1985 Volume 34 Issue 9 Pages T117-T122
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to generalize an automatic recrystallization method for preparing highly pure crystals, an improved apparatus was developed. The body of the extractor extremely simplified by a novel arrangement of a filter paper thimble was easy to make. A simple recrystallization flask, an effective porous glass boiling rod, and a high-heating-efficiency recrystallization heater were also easy to make and were based on the crystallization theory. A safety device for water and electricity, which was easy to construct, was useful: suspension of water supply, a burst rubber hose, or an electricity failure, which are problems that accompany unattended operations, will automatically result in shutting off both the electrical appliances and the flow of cooling water. The whole process of the recrystallization of compounds was automatically, safely, and cleanly carried out in the practically sealed system. The crystallization conditions produced in the described apparatus by using practically insoluble solvents were obviously consistent with the crystallization theory. In other words, crystals separated slowly from the dilute solutions, and these separated crystals ripened and became purified. The high-purity recrystallization purification could be performed more easily by the proposed technique than by the conventional manual technique. The quite pure phenacetins were obtained from water at extremely high recoveries(98% for each recrystallization) by the repeated automatic recrystallizations without any troublesome manual procedure required in an ordinary recrystallization. Their melting points were equal to and higher than that of acetophenetidine which was a melting point standard of National Institute of Hygienic Sciences. The transparent extraction reservoir was helpful for finding the end stage of recrystallization. The safety controlled apparatus should be quite useful for the high-purity automatic recrystallization of compounds.View full abstractDownload PDF (1017K) -
Hidehiro DAIDOJI, Michio MATSUBARA1985 Volume 34 Issue 9 Pages T123-T127
Published: September 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSThe determination of rare earth elements, thorium, and uranium in mussel, ark shell, and coral was made by inductively coupled plasma atomic emission spectrometry(ICP-AES). Four samples of mussels, original mussles, and mussels powdered by the original standard method, were dissolved with a mixture of HNO3 and HClO4. For one part of the sample solution, coprecipitation by ferric hydroxide was applied. Analytical values obtained with and without coprecipitation showed good agreement. The sample solutions for shells and coral were prepared by acid decomposition, and the elements to be determined were separated from calcium by coprecipitation to eliminate spectral interference by calcium. Analytical values were obtained from the calibration curves made with standard solutions containing matrix components at concentrations similar to those for real samples solutions. The concentrations of rare earth elements, Th and U in sample solutions of mussel ranged from 0.001 μg/g to 0.2μg/g. The concentrations of rare earth elements and Th in mussel, shells, and coral are 2000 15000 times higher than those in sea water.View full abstractDownload PDF (643K) -
Ichiro KOSHIISHI, Toshio IMANARI1985 Volume 34 Issue 9 Pages T128-T132
Published: September 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMolybdenum blue methods for the determination of orthophosphate in biological materials are used widely, but suffer from disadvantages as follows: increase of absorbance with standing time after the reaction, interferences from labile phosphates and reducing substances, and low sensitivity. Therefore, molybdenum blue methods {Fiske-SubbaRow method, Taussky method, Lowry-Lopez method, and Mo(V)-Mo(VI) method} were evaluated with high performance liquid chromatographic technique for the separation and determination of reduced phosphomolybdates. Fiske-SubbaRow method, whose reaction product was two-electron reduced phosphomolybdate, was interfered from labile phosphates and reducing substances. The absorbance of reaction mixture increased with standing time after the addition of reagents. Taussky method, whose reaction product was two-electron reduced phosphomolybdate, was interfered from labile phosphates but not from reducing substances. Lowry-Lopez method, whose reaction products were two-electron reduced and four-electron reduced phosphomolybdate, was more or less interfered from labile phosphates. Mo(V)-Mo(VI) method, whose reaction product was four-electron reduced phosphomolybdate, was sensitive but was interfered from labile phosphates. For the determination of orthophosphate in biological materials, it is necessary to choose a suitable method from molybdenum blue methods proposed by many workers.View full abstractDownload PDF (551K)
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