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Volume 27, Issue 10
Displaying 1-16 of 16 articles from this issue
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Takashi YAMASHIGE, Yukisato OHMOTO, Yasumasa SHIGETOMI1978 Volume 27 Issue 10 Pages 607-611
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThis method consisted of the consecutive three stages of procedure, i.e., the separation of selenium with a column of cation exchange resin, the conversion of selenium(IV) to hydrogen selenide with a pellet of zinc powder and binder, and the sweeping of selenide into a quartz cell of atomic absorption spectrophotometer. A given amount of particulate samples was gently heated in concentrated nitric acid together with a small amount of hydrogen peroxide in a water bath. After removing the insoluble residue, the solution was evaporated to dryness. The residue was taken up into 0.05 mol/l nitric acid, and introduced into a column φ 0.8×12cm, packed with Dowex 50WX8 {(50 100)mesh} in the hydrogen form. The effluent was evaporated to remove nitric acid and the residue was dissolved in 25 ml of 3.5 mol/l hydrochloric acid. The solution containing less than 1 μg of selenium was put into a reaction vessel, a pellet of zinc was added and the solution was covered tightly with the plunger. When the pressure guage reached 0.5 kg/cm2, hydrogen selenide evolved was carried away into the cell with nitrogen carrier. Selenium ranging from 0.1 to 5μg was determined in this way with a error of 3 %. Without the separation by ion exchange, copper, and chromium much interfered with the determination.View full abstractDownload PDF (854K) -
Sakingo IMAI1978 Volume 27 Issue 10 Pages 611-615
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSRecentry, the low temperature plasma ashing method has been employed as a decomposition method of organic materials for elementary analysis. The method is applied for biological, food, and environmental samples such as airborne particulates which are collected on membrane filter. In this paper, the recovery for 25 elements in low temperature plasma ashing method was investigated by activation analysis. The samples used in this experiments were prepared as follows. 100μl of 1000 ppm standard solution for each element was dropped on membrane filter or cellulose filter. Two mg of Mg or Fe as coexisting material was added thereto subsequently. In addition, samples were also prepared by adding 100μl of 1 M NH4Cl or 1M KCl solution to the above samples. Then, all samples were dried with an infra-red lamp in a dust-free box. A pair of the same sample was prepared. One of them was ashed and the other one was used, without ashing, for reference in activation analysis. The neutron irradiation was made for 1 min, 10 min or 1 h using the pneumatic tube system in Research Reactor Institute Kyoto University at a thermal neutron flux of 2.3 × 1013 n cm-2 s-1. Radioactivity measurements were made with a 30 cm3 coaxial Ge(Li) detector coupled to a ND-1024 channel pulse-height analyzer. The recoveries of As(III), As(V), Cd, Se(IV) and Se(VI), were found to be 55% to 94% in the presence of Mg(NO3)2 or FeCl3, whereas those of the other elements except for Hg, Br, and I, were found to be more than 95% under the same conditions. In the case of coexistence of NH4Cl, the loss of As(V), Cd, Cr, Fe, and Sb was slightly increased.View full abstractDownload PDF (966K) -
Masahide KAWANO, Tadaaki WAKIMOTO, Ryo TATSUKAWA1978 Volume 27 Issue 10 Pages 616-621
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for simultaneous determination of ethanolamines and N-nitrosodiethanolamine in commercial cutting fluids was developed. The procedure is as follows. A sample (about 10 mg) is taken into a test tube with a cap and then ethanol(1 ml), urea (2%, 0.5 ml) and acetic acid (0.1 ml) are added to it for destroying nitrite which is generally present in a sample. After being shaken slowly, the mixture is dried up by heating under the stream of nitrogen gas. Ethanol (about 1 ml) is added to the residue and dried up again. The residue is dried till it does not smell of acetic acid, and is silylated with dimethylformamide (200μl) and N, O-bis (trimethylsilyl)-trifluoroacetamide (200μl) at 60°C in an oil bath for 10 min. The silylated solution is diluted with dimethylchloride and an aliquot is injected into the GC-FID or GC-MS-MID. Selected mass numbers(m/e) of ethanolamines (mono, di and tri) and N-nitrosodiethanolamine are 102, 130, 262 and 130, respectively. Through the analytical process, artifact formation of N-nitrosodiethanolamine was notobserved. The detection limit for ethanolamines (mono, di and tri) and N-nitrosodiethanolamine by mass fragmentography were 1, 1, 1 and 5 ng and by gas chromatography were 4, 2, 2 and 4μg, respectively.View full abstractDownload PDF (977K) -
Tatsuru SASAGAWA, Tsuneo OKUYAMA1978 Volume 27 Issue 10 Pages 621-625
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the purpose of separation and analysis of peptides by high speed liquid column chromatography using volatile eluents, the effects of pH and polarity of eluents on retention of amino acids on octyl-silica were investigated. The use of lower pH eluents resulted in the increase of retention time. The ratio of capacity factor of an amino acid at pH 2.3 to pH 3.3 and at pH 10.3 to pH 3.3 were 7.3 and 0.1 respectively. The use of lower polar eluents such as 50% MeOH-0.01 M formic acid resulted in the reduction of retention time of hydrophobic amino acids, on the contrary in the increase of retention time of hydrophilic amino acids. Logarithmic plot of partition coefficient (of amino acids in octanol-water system) against the capacity factor gives a straight line with several eluents. In order to increase the affinity of rather polar substances, introduction of some substitutional groups gave some improvements. The ratios of capacity factor of an amino acid against its derivatives indicates a constant value φ which is specific for the substitutional group. Value φ is 2, 3, or 21 for N-glycyl, O-methyl, or N-acetyl, respectively. The retention time of peptides could be predicted from summation of the logarithm of capacity factor of each constitutional amino acid, using Pardee equation. On the other hand, from retention time of peptide and from the amino acid composition, molecular weight of a peptide was calculated. This method was successfully applied to an acidic peptide purified from bovine brain, and the peptide was assigned to be γ-glutamyl-cystinyl-glycine.View full abstractDownload PDF (910K) -
Norio FUKUSHI1978 Volume 27 Issue 10 Pages 626-630
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA test solution in a 50-ml measuring flask contained the following reagents, 5 ml of 1 M KCl as a supporting electrolyte, 10 ml of NH4Cl-NH3 buffer solution (pH 810), 05 ml of 10-2M H3BO3, and (15) ml of 10-3M of a polyphenol, such as Pyrocatechol Violet (PV), Pyrogallol Red, Bromopyrogallol Red. Difference between the oscillopolarograms of the solutions containing and not containing boric acid together with certain amounts of a polyphenol was only the variation of the peak currents based on the electrode reaction of the polyphenol, being accompanied with some variation in their peak currents with time elapsed. In the case of using PV as the polyphenol, the relation between the concentration of PV and the peak current was quantitative at the peak potential of -0.69 V vs. SCE. The decrease of the peak current (Δip) by the addition of boric acid in various concentrations was measured. To this procedure, the concentration ratio of PV to boric acid must be considered, too. Results obtained under various experimental conditions showed that an indirect determination of boron by oscillographic polarographic method is very promising.View full abstractDownload PDF (781K) -
Yusuke UJIHIRA, Matashige OHYABU, Tetsuro MURAKAMI, Tsuyoshi HORIE1978 Volume 27 Issue 10 Pages 631-636
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChemical states of iron(III) compounds, precipitated homogeneously by heating the iron(III) salt solution at 363 K in the presence of urea, was studied by menas of Mossbauer spectrometry and X-ray diffractometry. The pH-time relation of urea hydrolysis revealed that the precipitation process from homogeneous solution is identical to the hydrolysis of iron(III) ion at pH around 2 under the homogeneous supply of OH-ion, which is generated by hydrolysis of urea. Accordingly, iron(III) oxide hydroxide or similar compounds to the hydrolysis products of iron(III) ion was precipitated by the precipitation from homogeneous solution methods. Akaganeite (β-FeOOH) was crystallised from 0.1 M iron(III) chloride solution. Goethite(α-FeOOH) and hematite (α-Fe2O3) was precipitated from 0.1 M iron(III) nitrate solution, vigorous liberation of OH- ion favoring the crystallization of hematite. The addition of chloride ion to the solution resulted in the formation of akaganeite. Basic salt of iron sulfate[NH4Fe3(OH)6 (SO4)2] and goethite were formed from 0.1 M iron(III) sulfate solution, the former being obtained in the more moderate condition of the urea hydrolysis (<363 K) and the latter being produced in the more vigorous hydrolysis condition of urea (>363K).View full abstractDownload PDF (890K) -
Naobumi OI, Ko-ichi MORIGUCHI, Mari MATSUDA, Hiro-o SHIMADA, Osamu HIR ...1978 Volume 27 Issue 10 Pages 637-641
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSN-Acyl amino acid esters are the typical optically active stationary phase for gas chromatographic separation of amine enantiomers, and carbonyl-bis-(aminoacid esters) are the useful phases for the separation of amine enantiomers. However, these phases suffer from relatively high column bleeding which limits the working temperature to 110°C and 125°C, respectively. In order to overcome this disadvantage, we prepared some new s-triazine derivatives of amino acid esters. It was found that these new phases give good properties in relation to enantiomer separation and thermal stability. For example, N, N', N''-[2, 4, 6-(1, 3, 5-triazine] trilyl)-tris-(L-valine isopropyl ester) exhibits excellent property for the separation of both amino acid and amine enantiomers. Moreover, its maximum permissible operating temperature (about 150°C) is considerablly higher than those of all published phases containing amino acid ester groups. Its low melting point {(6768)°C (uncorr.)} is also convenient which enables the column to be used over a larger temperature range. It is very noticeable that these new stationary phases, which have no-CO-NH-groups, give essentially the same separation as N-acyl amino acid esters or carbonyl-bis-(amino acid esters). This fact siggests that -N=C-NH-C- groups make a contribution to resolution of enantiomers in these new phases.View full abstractDownload PDF (752K) -
Takeshi NAGANUMA1978 Volume 27 Issue 10 Pages 641-645
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPyronine G reacts with mercury in hydrobromic acid medium to form a Pyronine G-mercury complex with reddish orange fluorescenece, and was used as a reagent for the fluorometric determination of mercury. The kind of acids and solvents, concentration of acid and reagent and the effect of diverse ions were investigated. For the determination of mercury, 1.0 ml of 0.3% Pyronine G solution was added to the sample solution containing (0.11.0)μg of mercury, and the acid concentration was adjusted to (0.010.03)N in hydrobromic acid (final volume: 5 ml). The Pyronine G-mercury complex was extracted with 5 ml of butyl acetate, benzene + acetone or toluene + acetone. The organic phase was separated and centrifuged, and its fluorescence (ex. 365 nm, fl. 580 nm) was measured against the reference Rhodamine B solution (0.2 μg/ml). Au(III) and Cr(VI) interfered. The method is simple and accurate for the determination of mercury. The limit of determination was 0.05μg Hg/ml in benzene-acetone mixed solvent.View full abstractDownload PDF (833K) -
Akio FUJIWARA, Kunihiro WATANABE, Kyozo KAWAGAKI1978 Volume 27 Issue 10 Pages 645-650
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe solvent extraction-spectrophotometric determination of indium and gallium with salicylideneamino-2-thiophenol (SATP) was studied. Indium reacts with SATP in the presence of ο-phenanthroline(ο-phen) to form a ternary complex, which can be extracted quantitatively into chloroform. Under the optimum conditions Beer's law holds up to 160 μg of indium, and up to 40 μg of gallium in 10 ml of chloroform, respectively. When the pH's of the aqueous phase were in the range of 4.66.0 for the indium ternary complex and 4.55.8 for the gallium chelate, a constant absorbance was obtained, and extractability was greater than 99% for the indium ternary complex. Many elements interfered with the determination of indium and gallium. Silver was masked with thiourea, and gold masked with L-ascorbic acid. Vanadium and gallium were masked by tartaric acid. However, copper and palladium must be removed before analysis. The standard procedure is as follows: Take (1030) ml of a sample solution containing less than 160 μg of indium. Add 1 ml of a buffer solution (1 M acetic acid and 1 M sodium acetate) and 3 ml of a 0.1% ο-phen solution. Adjust the pH to 5.0. Then add 1 ml of a 0.1% SATP (ethanolic solution) and dilute to about 50 ml with water. Extract the indium complex with 10 ml of chloroform by shaking for 3 min. Measure the absorbance of chloroform phase at 425 nm (the molar absorption coefficient, 1.1 × 104 1 mol-1 cm-1).View full abstractDownload PDF (985K) -
Kazuhiro KUWATA1978 Volume 27 Issue 10 Pages 650-655
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and sensitive mass spectrometric analysis was developed to determine chrysene (Chrs.) and benzopyrene (BP) in the atmospheric environment. Airborne particulate was sampled on a glass fiber filter by a high-volume air sampler for (124) h and extracted for 5 h with 50 ml of cyclohexane in a soxhlet extractor. The extract was reduced to 5 ml by evaporation in a Kuderna-Danish apparatus. Five μl of the solution was taken into a sampling probe with glass fiber filters in it and 2 μl of an internal standard solution containing 100 ng of benzanthrone (molecular weight 234) was added. The sampling probe was dried at room temperature for 2 min and then inserted into the ionization chamber of a mass spectrometer. Ion currents of m/e 228, m/e 252 and m/e 234 were measured every 30 seconds by the mass spectrometer. Amounts of Chrs. and BP in the extract were calculated from integrated ion currents of m/e 228 and m/e 252 relative to m/e 234. Working conditions of the mass spectrometer were as follows: ionization voltage 70 eV, total emission 80 mA, vacuum (56) × 10-7 mmHg, temperature of the ionization chamber 80°C, scan range m/e 226254. Determined values of Chrs. and BP by the mass spectrometry were required to be corrected by multiplying the value of Chrs. by 0.953 and by multiplying the value of BP by 0.693 in the case of ambient air in Osaka because they were affected by isomers of Chrs. and BP contained in airborne particulate. Advantages of the technique were high sensitivity, excellent quantitative accuracy and simple analytical procedure. Relative standard deviations of measured values of Chrs. and BP in the range of (0.150)ng were (27)%, and analysis time of the mass spectrometry was (78)min per a sample.View full abstractDownload PDF (1043K) -
Toshio YAO, Tamotsu WASA, Soichiro MUSHA1978 Volume 27 Issue 10 Pages 655-659
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn electroanalytical method was proposed for the determination of four constituent bases (guanine, adenine, thymine, and cytosine), which are important components of deoxyribonucleic acids (DNA). When DNA {(5100)mg} was hydrolyzed by boiling on a water-bath for 80 min in 4 ml of 70% HClO4, the bases were released from DNA molecules quantitatively. Guanine, adenine, and thymine were voltammetrically oxidized at a glassy carbon electrode, and each of them gave a well-defined oxidation peak at different potentials over the pH range of 012. Consequently, it was possible to determine simultaneously three bases in hydrolyzed solution of DNA, by using Britton-Robinson buffer in the pH range of 24 as a supporting electrolyte. Also cytosine was able to determine by polarography with a dropping mercury electrode, by using Britton-Robinson buffer at pH 9.5 as a supporting electrolyte. Deoxyribose and phosphate, which are other components of DNA, were electro-inactive, and did not interfere with the determination of these bases. The proposed method was simple and rapid, since no time-consuming separation techniques were required.View full abstractDownload PDF (777K) -
Masayuki SETO1978 Volume 27 Issue 10 Pages 660-663
Published: 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA sample water treated by phosphoric acid in the oxidation vessel was bubbled by carbon-free air to expel the inorganic carbon, and was heated to produce carbon dioxide from organic materials by potassium persulfate oxidation using silver nitrate catalyzer. After the removal of water vapor by desiccant, the concentration of carbon dioxide was measured by nondispersive infrared gas analyzer. The calibration curve was linear over the range of 0.5 to 5000 μg C in l to 50 ml of glucose standard solution. The coefficient of variation of 10 replicates of 100 μg C glucose was 1.6%. It was also ascertanied that the method was applicable not only to the dissolved organic compounds but also for the particulated matter of small organisms. The method is valid for the determination of TOG in natural waters and for the rapid monitoring of organic pollutants in water-works and sewers.View full abstractDownload PDF (594K) -
Tatsuhiko TANAKA, Takayoshi YOSHIMORI1978 Volume 27 Issue 10 Pages 664-666
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe stability of dilute standard solutions of nitric acid (M/1000 and M/200) was investigated for a period of more than two years by coulometric titration. The bottles made from soft glass, Pyrex, low-density polyethylene and Teflon, and also quartz Erlenmeyer flasks were tested as their containers of the solutions. Prior to use, these containers were filled with 1:1 nitric acid for a day and rinsed thoroughly with deionized water and then with distilled water. The concentrations of the solutions stored in polyethylene, Teflon and quartz containers did not change more than two years. A serious decreases of acidities could be found for the standard solutions stored in the soft glass containers. The decreases after about two and a half years were about 97 and 12% in M/1000 and M/200 solutions, respectively. The acidity of M/1000 solution in Pyrex bottle also decreased during long storage (about 3%/2.5 y). The main source of these decreases is attributed to neutralization of some alkaline materials from the glass containers. Teflon and quartz are advisable as the best container materials. Polyethylene bottle is also suitable for the storage of dilute standard solution of nitric acid. Amount of carbon dioxide, which permeated through the plastic containers and was absorbed by the solution, was also measured and was nearly the same as that of the equilibrium concentration of the dioxide in water or dilute acid solution exposed in air.View full abstractDownload PDF (526K) -
Takao MITSUHASHI, Hideyoshi MORITA, Shigeru SHIMOMURA1978 Volume 27 Issue 10 Pages 666-668
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSOrganic mercury compounds such as methylmercury (II) chloride (MMC) and phenylmercury(II) acetate (PMA) were decomposed and reduced by a combined Fe(II)-or Fe(III)-NaBH4 reagent. A new method utilizing this phenomenon for the determination of mercury in solution by a cold vapor atomic absorption technique is described. A closed type cell (light path length: 10 cm) equipped with a reaction vessel was used for a device. The procedure is as follows. 150 ml of sample solution containing (0.151.05)μg as mercury was taken into a reaction vessel. After the vessel was connected with the closed type cell, 1.5 ml of Fe(II) or Fe(III) (1.00×103 ppm) and 1 ml of NaBH4 {1% (w/v)} solutions were added to the vessel through an upward inlet of the cell, and then the inlet was closed immediately with a stopcock. Then the absorbance due to vaporized mercury atoms was measured until the highest absorption peak was obtained. The addition of Fe(III) was more effective for the determination of organic mercury than that of Fe(II). The linear standard curves for MMC and PMA (as well as HgCl2) were obtained by the method using a combined Fe(III)-NaBH4 reagent. The detection limit (S/N=2) for mercury was down to 0.1 ng/ml.
The application of this method is expected for the determination of total mercury and for the selective determination of inorganic and organic mercury in natural water samples.View full abstractDownload PDF (456K) -
Kyoji TÔEI, Shoji MOTOMIZU, Shoichi HAMADA1978 Volume 27 Issue 10 Pages 668-671
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS2-Nitroso-5-diethylaminophenol (nitroso-DEAP) reacts with palladium to form the red complex in acidic solution {(27) N H2SO4}. This complex is quite soluble in aqueous acidic solution and is very stable. Analytical-procedure is as follows. Transfer the sample solution containing about 30 μg or less of Pd(II), to a 10 ml volumetric flask. Add 3 ml of 15 N sulfuric acid and 1 ml of nitroso-DEAP aqueous solution (6×10-3 M in 0.1 N H2SO4). Dilute it to 10 ml with distilled water. After standing for about 5 min, measure the absorbance at 540 nm. The molar absorptivity of the complex at 540 nm is 2.33×104 l mol-1 cm-1, and the absorbance of the reagent blank is 0.013±0.002. The composition of the complex is metal: ligand=1:2, and the complex does not decompose for at least 3 days. Less than 10-2M of K+, Na+, NO3- and Cl-, less than 10-3M of Mg2+, Ca2+, Zn2+, Cd2+, Fe3+, Co2+, Ni2+, Cu2+, Hg2+, Mo(VI), U(VI), Al3+, Cr3+ and Br-, less than 10-4M of Rh(III), Pt(IV), Zr(IV), Mn2+ and Sn4+, less than 5×10-6M of W(VI) and less than 10-6M of Sn2+ do not interfere with the analysis. By this procedure, palladium in catalyst for the clarifier of car waste gas was determined.View full abstractDownload PDF (635K) -
Norio ICHINOSE1978 Volume 27 Issue 10 Pages 671-673
Published: 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe procedure is as follows: Twenty-five ml of 0.25 N nitric acid solution containing phosphoric and silicic acids is heated in a water bath of about 60°C. One ml of 5% ammonium molybdate is added to the solution, and the mixture is allowed to stand further for 5 min in the water bath. By this process, the molybdoheteropoly acid is formed. After cooling to room temperature, the aqueous solution is transferred into a separatory funnel together with 5 ml of methyl propionate. Molybdophosphoric acid is selectively extracted into the organic phase by shaking for 10 min. Then the aqueous phase is equilibrated with 5 ml of methyl isobutyl ketone. By this process, molybdosilicic acid is extracted into the organic phase. After centrifuging to remove water suspended in the both organic phases, the molybdoheteropoly acid is determined by high-speed liquid chromatography with a ultra-violet spectrophotometric detector. Phosphoric acid ranging from (0.0150.2) ppm (as phosphorus) and silicic acid ranging from (0.152) ppm (as silicon) in aqueous solution can be determined rapidly by this method.View full abstractDownload PDF (439K)
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