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Volume 34, Issue 4
Displaying 1-16 of 16 articles from this issue
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Toshihiko KADOYA, Katsuko FUKUMOTO, Takashi MANABE, Tsuneo OKUYAMA1985 Volume 34 Issue 4 Pages 151-156
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSFor the rapid analysis of a large number of protein samples, an analytical system using micro-slab polyacrylamide gel electrophoresis was developed. Two sizes of gels were employed, one (38 × 37 × 0.5mm) for 10 samples and the other (38 × 100 × 0.5mm) for 25 samples. Twenty six slab gels for 10 samples or 8 slab gels for 25 samples were prepared in a gel casting chamber in a time. Eighty samples (8 slab gels for 10 samples) or 100 samples (4 slab gels for 25 samples) were analyzed in parallel in one cycle. A piece of filter paper covered by a stainless steel plate was used as a bridge between the buffer on a slab gel and that in the cathode chamber. Electrophoresis was performed at a constant current of 40mA per slab gel for 4min. The gels were stained in 0.1% Coomassie Brilliant Blue R-250 in a mixture of methanol, acetic acid and water (50 : 7 : 43, by volume) for 3 min and destained in 7% acetic acid for 5 min. For the detection of very small quantity of proteins (500 pg), the gels were silver-stained within 15 min. Overall standard analysis time of the present method was 30 min including setting of gel molds, application of samples, electrophoretic run and Coomassie Blue staining. Quantitative analysis of the stained protein bands was performed by television camera-microcomputer system.View full abstractDownload PDF (1006K) -
Kazue TANI, Yoshihito SUZUKI1985 Volume 34 Issue 4 Pages 156-161
Published: April 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSThe behavior of chromatographic retention was investigated thermodynamically for two kinds of derivatives with two aqueous-organic mobile phases; methanol and acetonitrile. The derivatives used were aliphatic saturated aldehydes from methanal to heptanal and their isomeric ketones, which were converted to the corresponding 2, 4-dinitrophenylhydrazones and 1-dimethylaminonaphthalene-5-sulfonylhydrazones, respectively. Thermodynamic properties of solutions were examined as a function of eluent composition. Enthalpies and entropies of transfer were calculated from retention data by evaluation of Van't Hoff plots. For all cases examined, the enthalpies of transfer were negative and increased with the concentration of organic modifier in the eluent. The entropies of transfer increased with increasing the concentration of methanol. With the increase in acetonitrile concentration, on the other hand, the entropies of transfer tended to decrease as the carbon numbers of both derivatives increased. This tendency suggested the existence of direct interaction between the bonded hydrocarbon chain and alkyl chains of derivatives. The bonded hydrocarbon chain in aqueous acetonitrile mobile phase seemed to be pictured as an alkyl 'brush', whose individual bristles made up the surface with which the solute molecules in the mobile phase interacted. The bonded hydrocarbon chain in aqueous methanol mobile phase seemed to form 'liquid-droplet'-like phase, which behaved as a liquid with the analogous liquid-liquid partitioning systems.View full abstractDownload PDF (997K) -
Shigehisa KOMIYAMA, Yoshio YAMAURA, Hiroyuki NAKAZAWA, Masahiko FUJITA ...1985 Volume 34 Issue 4 Pages 161-165
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSimultaneous determination of ibotenic acid and muscimol in Amanita muscaria has been developed by means of high performance liquid chromatography. The extracts of mushroom with 50% methanol were poured onto a Dowex 1-X8 column (acetate form). Ibotenic acid was adsorbed and muscimol passed through the column. After concentration of the fraction containing muscimol, it was added on the bi-layer column (upper : alumina, lower : silica gel) and eluted with acetone-methanol-water (2 : 2 : 1). Ibotenic acid was eluted with 0.1M acetic acid from the Dowex 1-X8 column. Both effluents were combined and evaporated to dryness at 40°C. The residue was dissolved in 1ml of 50% methanol and injected into a Shim-pack P NH2-10/S2504 column (10μm, 4.0 x 250mm) at 40°C. The sufficient resolution was obtained using 0.01M phosphate buffer (pH 4.5)-methanol (30 : 70) as mobile phase with the flow rate of 1.0ml/min and detected at 220nm. The recovery for ibotenic acid and muscimol were 99.3% and 90.6%, respectively. The method can be applicable for the determination of ibotenic acid and muscimol in poisonous mushroom such as A. muscaria with determination limit of 18 and 10ppm, respectively.View full abstractDownload PDF (782K) -
Yoshinori UWAMINO, Toshio ISHIZUKA, Akira TSUGE, Hideo YAMATERA1985 Volume 34 Issue 4 Pages 166-170
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIndividual rare-earth (RE) oxides in light RE oxide mixtures were analyzed by X-ray photoelectron spectrometry. The spectral intensities of respective elements were measured as the total area of the RE3d5/2 peaks and the satellites. For cerium the peak area in the energy range of 910894 eV was taken as the intensity. The detection limits ranged from 1.4 to 3.6wt%. The amount of lanthanum oxide in the samples was determined by the method of standard addition. For other oxides calibration curves were made by using a fixed amount of lanthanum added to the samples as an internal standard. The amounts of the oxides were determined from the spectral intensities relative to the lanthanum intensity and the concentration of lanthanum oxide. The relative error in the analytical values for synthetic samples was less than 10 % with a few exceptions. The analytical values for real samples showed a reasonable agreement with those determined by inductively coupled plasma emission spectrometry.View full abstractDownload PDF (1016K) -
Yasuo INOKUMA, Hirofumi KURAYASU1985 Volume 34 Issue 4 Pages 170-174
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe present method was studied to get accurate value of the 10-4% order in the determination of phosphorus from 1 to 100ppm in iron and steel. The sample (1g) is decomposed by heating in HCl-HNO3. Phosphorus is oxidized to phosphate by white-fume treatment with HClO4. The treated sample is adjusted by water to a 100ml. A 1/5 sample aliquot (20ml) is taken. The phosphomolybdate (MPA) formed in 6 M HNO3solution is extracted into isobutyl acetate (20ml) and then back-extracted into a 10ml HCl solution (1.2M) with SnCl2solution (0.26M) and reduced to molybdenum-blue. The absorbance of this solution is measured at 940nm against distilled water as reference. The absorption maximum at 940nm besides 700nm was newly observed in the absorption curve of this molybdenum-blue. The apparent molar absorptivity of the former peak was 1.6 x 104l mol-1cm-1and about 1.3 times as large as that of the latter. The absorbance of the reagent blank was less than 0.01 against distilled water as reference. Arsenic and silicon, which are considered to form heteropoly acids as well as phosphorus, and niobium, vanadium, and zirconium, which form heteropoly acids by reaction with MPA interferred seriously. But MPA could be completely free from interference of heteropoly acids of arsenic and silicon by resulting in the formation of acid solution and then extracting into isobutyl acetate. By the same fashion, the interference of niobium, vanadium, or zirconium could be also suppressed by forming MPA in HNO3solution above 5 M. The following elements did not interfere up to 50% Cr, 10% Ni, 0.5% of Nb, Si, Ti, V, and Zr, 0.2% W, and 0.05% As. The relative standard deviations were 28% for 10100ppm in iron and steel. The present method is good for getting accurate value of the 10-4% order in the determination of phosphorous between 1 and 100ppm in iron and steel because of widely measuring range and simple procedure.View full abstractDownload PDF (915K) -
Yoshifumi HARADA, Natsuko KURATA1985 Volume 34 Issue 4 Pages 175-179
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA coprecipitation technique was investigated for the separation and concentration of titanium, vanadium and zirconium in aluminum. Lanthanum hydroxide was employed as the collector, and the elements were determined by inductively coupled plasma emission spectrometry (ICP-ES). Aluminum sample (1g) was dissolved on heating with hydrochloric acid and then nitric acid. After the addition of lanthanum ion (La : 20mg), a sodium hydroxide solution was added to form lanthanum hydroxide, while aluminum was dissolved as Al(OH)4-. The analyte elements were coprecipitated with lanthanum hydroxide. The precipitate was separated by filtration and dissolved with dilute hydrochloric acid. The solution was made finally to 25ml with water and sprayed into the ICP. The emission intensities at 334.94nm (Ti), 310.23nm (V), and 343.82nm (Zr) were measured for the determination of the elements. The emission intensity of zirconium decreased with the concentration of aluminum in the sample solution (above 50μg Al/ml), presumably because of interference in plasma from aluminum. The observed content of zirconium was corrected by determining aluminum in the solution (about 200μg Al/ml) by ICP-ES. We presumed that vanadium was coprecipitated as LaV4O9OH·χH2O with lanthanum hydroxide. The coefficients of variation for the elements at 25ppm in aluminum were all about 1%. It was confirmed that other elements (Fe, Cu, Mn, Cr, Ni and Cd) were also quantitively separated with lanthanum hydroxide from aluminum. This method was applied for the determination of 150ppm levels of titanium, vanadium and zirconium and 11700ppm levels of other elements in aluminum samples.View full abstractDownload PDF (724K) -
Shigemitsu OKAZAKI, Hajime TAKIMOTO, Yoshihito SUZUKI1985 Volume 34 Issue 4 Pages 180-183
Published: April 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSThis study was performed to develop a detector for micro high performance liquid chromatography (HPLC) or semimicro HPLC, which could theoretically detect all eluates with high sensitivity. All of the eluent from HPLC column was absorbed on the surface of a fused quartz rod covered with the porous powder of diatomaceous earth by the electrospray method. The solvent was then removed, and the remaining sample on the rod was detected by the hydrogen flame ionization method. The rod was prepared as follows. The mixture of porous diatomaceous earth (140μm, particle size) and glass powder was deposited on the rod (0.9mm o.d.) by the half melting method. The rod was then dipped in a silver nitrate solution to make it electrically conductive and was dried by passing it through the hydrogen flame in the detector. By applying electric potential (3.5 kV) between the electrospray-nozzle and the rod, the eluent of HPLC was nebulized from the nozzle (0.12mm i.d.) on the rod. The separation of p-bromophenacyl esters of carboxylic acid could be achieved on ODS-micro column (0.5mm i.d., 16.5cm in length) with 80% methanol-water as a mobile phase. The shapes of peaks on chromatograms were the same as those obtained by the UV-detection method.View full abstractDownload PDF (616K) -
Teruo HINOUE, Michiko ITOH, Hidemi KIKUCHI, Hideo MURATA, Yu YOKOYAMA1985 Volume 34 Issue 4 Pages 183-188
Published: April 05, 1985
Released on J-STAGE: November 18, 2010
JOURNAL FREE ACCESSIn cathodic stripping voltammetric determination of uranyl ion with trioctylphospine oxide (TOPO), the use of a hanging mercury drop electrode (HMDE) fairly simplifies the analytical procedure compared with that of a glassy carbon electrode. However, when the cathodic stripping voltammetry with HMDE is applied to the determination of trace amounts of uranium in brines from natural gas fields, it gives no reliable results, showing low peak heights and low reproducibility. From the results of the cathodic stripping voltammetry of uranyl ion in various electrolyte solutions, it was found that the addition of a large amount of nitrate ion as a supporting electrolyte enhanced the peak height of uranium and showed good reproducibility. On the basis of the results of uranyl ion extraction into cyclohexane containing TOPO, it was concluded that the effect of supporting electrolytes on the voltammetry of uranium was attributed to the complex formation of uranyl ion with electrolyte anions in the solutions. By using this improved procedure, uranium in sea water was determined to be 3.4 ppb. The procedure was also applied to the determination of uranium in brines from some natural gas fields.View full abstractDownload PDF (1099K) -
Hiroaki TAO, Akira MIYAZAKI, Kenji BANSHO1985 Volume 34 Issue 4 Pages 188-192
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe hydride generation technique is quite effective for improving the detection limit of tin in atomic absorption spectrometry. However, there are some difficulties such as the very narrow acidity range for stannane generation, the serious interference from diverse ions, and the reagent blank which actually determine the detection limit of tin. To overcome these difficulties, several inorganic and organic acids have been used as the reaction media to reduce tin to stannane, but buffer solutions have been scarcely used so far. The aim of this paper is to examine the effect of acidity and diverse ions of the reaction media on the stannane generation particularly at the pH range from 3 to 7 with CH3COOH-CH3COONa and tris(hydroxymethyl)aminomethane-HCl buffer solutions. Stannane was generated by the reduction of tin in buffered reaction media with sodium borohydride, condensed in a liquid nitrogen trap and subsequently introduced into nitrogen-hydrogen flame for atomization. The reduction of tin with sodium borohydride was more efficient for the solution at higher pH value. The minimal amounts of sodium borohydride for the complete generation of stannane in the buffer solutions at pH 3.2 and pH 7.0 were about 2/5 and 1/10, respectively, compared with that of 0.1M HCl solution. In addition, since the reagent blank of tin due to these buffer solutions could be easily removed as the hydride before use, the total reagent blank of tin could be lowered to about 1/5 and 1/20 of that for 0.1M HCl solution, respectively. The minimal detectable amounts of tin was 0.3ng with the present procedure. Interferences from transition metals such as Fe, Cu, Co and Ni were reduced in CH3COOH-CH3COONa buffer solution at pH 3.2. For example, the presence of Fe at the concentration level of 106-fold ratio to Sn gave no interference. As an application, this buffer solution was used for the determination of tin in standard steel samples (JSS 420-1 and NBS 19G). The results obtained were in good agreement with the certified values.View full abstractDownload PDF (806K) -
Shigeroku YAMAGUCHI, Katsuya UESUGI1985 Volume 34 Issue 4 Pages 193-196
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn extraction-spectrophotometric method for the determination of gold using 2-hydroxy-1-naphthaldehyde-4-phenyl-3-thiosemicarbazone (HNA·PS) was studied. The method is based on the formation of an insoluble gold(III)-HNA·PS complex, which is extractable into ethylacetate from acidic solutions. The gold(III)-HNA·PS complex in ethylacetate exhibits a maximum absorption at 446nm with apparent molar absorption coefficient of 2.08×104dm3mol-1cm-1. Under the optimum conditions Beer's law is obeyed up to 100μg of gold(III) in 10cm3of ethylacetate. For 50μg of gold(III), the coefficient of variation was 0.92 % in 6 determinations. The recommended procedure is as follows: take an aliquot of sample solution containing up to 100μg of gold(III) into a 50cm3-separatory funnel. Add 7.5 cm3of 3 mol dm-3 sulfuric acid solution, and dilute with water to about 30 cm3(0.75 mol dm-3). Then add 10cm3 of 2.5×10-4mol dm-3 HNA·PS ethylacetate solution and shake vigorously for 10min. Filter the organic phase through a dry filter paper and measure the absorbance at 446nm against reagent blank. By this method the gold(III) in the presence of 500μg of silver(I), cobalt(II), iron(III), mercury(II), iridium(III), nickel(II), platinum(IV), titanium(IV) and vanadium(V) can be determined, although palladium(II) seriously interfered. The method is simple, convenient and reproducible.View full abstractDownload PDF (582K) -
Tatsuya KISHIMOTO, Yasuaki SHIMOISHI, Kyoji TÔEI1985 Volume 34 Issue 4 Pages 197-199
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA new reagent, 1-methylamino-2-amino-4, 6-dibromobenzene (MADB) for the gas chromatographic determination of ultramicro amounts of nitrite ion was synthesized. It reacts with nitrite ion to form 1-methyl5, 7-dibromobenzotriazole(MDBT) which can be extracted into toluene. The extract is very sensitive to electron capture detection in gas chromatography. Therefore, the conditions for the gas chromatographic determination of ultramicro amounts of nitrite ion were investigated by using MADB. A typical procedure is as follows; Take the sample solution containing less than 60ng of nitrite ion into a 25ml of stoppered test tube and dilute to 15ml with distilled water. Add 2ml of concentrated hydrochloric acid and 0.5ml of MADB solution(2×10-4mol dm-3), and allow the mixture to stand for 30min. Extract the MDBT formed into 2ml of toluene by shaking for 5min, and wash the toluene extract with 4ml of 3mol dm-3hydrochloric acid. Inject 2μl of the toluene extract into gas chromatograph(ECD) and measure the peak height. The calibration curve(peak height) is linear in the range of 2.5 to 10ng of nitrite ion in 15ml of solution. The reproducibility at 3.5ng ml-1 was 3%. Trace nitrite ion in commercially available inorganic salts was determined by the proposed procedure.View full abstractDownload PDF (460K) -
Yutaka KANAI, Noboru IMAI, Shigeru TERASHIMA1985 Volume 34 Issue 4 Pages 199-202
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA rapid and precise method for the determination of trace amount of uranium in geological materials by trioctylphosphine oxide (TOPO) extraction-Arsenazo III spectrophotometry was presented. A sample (0.1 1 g) was decomposed with a mixture of HNO3-HClO4 HF, and evaporated to dryness. The residue was dissolved with (1+1) HNO3, and mixed with 2 % NaF solution and 10 % ascorbic acid solution, followed by addition of nitric acid up to 2 M concentration. Uranium was then extracted with 2 ml of 0.1 M TOPO-cyclohexane. The organic phase was washed twice with 2 M HNO3 containing NaF and ascorbic acid, and was mixed with Arsenazo III solution and butyl cellosolve. The absorbance of the admixture was measured at 653 nm using 5 cm cell. More than 0.2 ppm of uranium could be determined by the method and the relative standard deviation at 1 ppm uranium concentration was 13 %. Ten samples could be analyzed in 5 h. This method was applied satisfactorily to a variety of geological reference materials.View full abstractDownload PDF (719K) -
Ichiro TAKEDA1985 Volume 34 Issue 4 Pages 203-205
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSConcerning waste water from a laundry machine, a use of gas detector tube has been studied for the determination of tetrachloroethylene(TCE) in water. In a syringe method, 100 ml of water containing TCE and 108 ml of air are taken in a 200 ml glass syringe. After vigorous shaking, 100 ml of the equilibrated air is taken out to pass through a TCE gas detector tube. In a more simplified method, 200 ml of water containing TCE is taken in a 500 ml stoppered glass bottle. After shaking, 50 ml of the equilibrated air in a head space is passed through a detector tube by means of a disposable syringe. Concentration of TCE in water is then calculated by using Henry's constant determined in a separate experiment. The detection limit of a gas detector tube is 3 ppm, while a Henry's constant, expressed by ppm TCE in air/mg l-1TCE in water attains the value of about 70. Consequently the limit of detection of TCE in water is about 0.1 mg/l for the syringe method, and about 0.3 mg/l for the simplified bottle-equilibration method.View full abstractDownload PDF (548K) -
Keiichi FUKUSHI, Kazuo HIIRO1985 Volume 34 Issue 4 Pages 205-208
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSNew determination procedure of fluoride ion in sea water was developed with a capillary type isotachophoresis after coprecipitation enrichment by magnesium hydroxide. Using a capillary tube with 200mm in length and 0.5mm in inner diameter connected a PTFE tube with 80mm in length and 1.0mm in inner diameter, optimum electrolyte system was studied for the determination of fluoride ion. Fluoride ion could be determined successfully using the leading electrolyte containing 0.01 M histidine hydrochoride, 0.1 % Triton X-100 and the terminating electrolyte containing 0.01 M hexanoic acid. Effects of amount of sodium hydroxide solution for coprecipitating fluoride ion and of concentration of sodium hydroxide solution for washing precipitate on the recovery of fluoride ion were examined. As a result, a solution of 1.5ml of 1 M sodium hydroxide and 10-3 M sodium hydroxide solution were respectively found to be optimum for 50 ml of sample. One and a half milliliters of 1 M sodium hydroxide solution was added to 50ml of artificial sea water sample containing fluoride ion to enrich the ion with magnesium hydroxide. To prevent the interferences caused by anions of high concentration, centrifuged precipitate was washed with 10-3 M sodium hydroxide solution and dissolved by adding 1.3g of Dowex 50 W X8 ion exchange resin. The total volume was made to 5.0 ml with distilled water after filtration. A 50μl aliquot of the above solution was injected into the isotachophoresis apparatus. The linear working curve was obtained. The proposed method was applied to the determination of fluoride ion in the coastal sea water samples in Osaka Bay collected in April, 1984. The result obtained by the working curve method agreed closely with that obtained by the standard addition method.View full abstractDownload PDF (610K) -
Osamu NARA1985 Volume 34 Issue 4 Pages 208-211
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn automatic solid-liquid extraction apparatus was developed for rapid and exhaustive extraction. The extractor body was extremely simplified by the novel arrangement of a filter paper thimble. The number of joints is kept to a minimum. Wide filteration area, which is close to that in a regular soxhlet, was obtained and there was no flow resistance through the filter paper. A filter paper thimble is placed firmly between the filter plug and the socket by pressing down the plug on which the thimble has been placed. Contents in the extraction reservoir are heated exhaustively by the solvent vapor(e.g., at 79.5 °C in using water) and stirred in order to increase the extraction efficiency remarkably. Continuous flow of the condensed solvent agitated with the sample keeps a stable boiling, rather than batchwise as in a soxhlet. The present extractors with 11 ml and 57 ml of reservoir capacities were applied to crude fat extraction from ground soybean. The extractor with 11 ml capacity completed the extraction within 20 min., whereas the soxhlet with 72 ml capacity did not complete even in more than 90 min. The plain extraction reservoir is helpful for finding the end stage of extraction. The present apparatus is simple to be made, durable to be used, easy to be cleaned, and should be useful for the rapid and exhaustive solid-liquid extraction.View full abstractDownload PDF (858K) -
Masahiro HORI, Tsuyoshi FURUYA, Yoshitaka KOBAYASHI1985 Volume 34 Issue 4 Pages 211-214
Published: April 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method was investigated to evaluate the conversion efficiency of carbonyl halide into sym-diphenyl urea (DPU) without the measurement of recovery. The combustion gas of vinyl chloride monomer from a diffusion burner was used as a sample gas, and the gas was divided into two flows with almost the same flow rates of 0.4 l/min. These two flows were passed in parallel through two bubblers containing 20ml of aniline absorbing solution for 8 min at different sampling conditions, and DPU formed in the absorbing solution was determined by high performance liquid chromatography. When a condition in which carbonyl halide could be quantitatively converted into DPU would be adopted for one of the gas flows (A), the conversion efficiency in the condition for the other (B) could be evaluated from the ratio of analytical value of DPU of B to that of A. No difference could be detected between the conversion efficiencies with induction tube length of 20 and 40 cm. The efficiency and recovery was at a plateau(9497%) in the aniline concentration range of not less than 0.8 %. The residual gas after explosion of a mixed-gas containing trifluorobromomethane was also used as a sample, and similar results were obtained.View full abstractDownload PDF (685K)
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