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Volume 29, Issue 6
Displaying 1-16 of 16 articles from this issue
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Yoshiaki OKAJIMA, Yutaka FUKUI, Hideo TODOKORO, Yoshio SAKITANI1980 Volume 29 Issue 6 Pages 351-356
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA newly developed Auger electron spectrometer equipped with a field emission electron gun was used for the quantitative analyses of carbides in 25Cr-20Ni casting steel containing 0.4% titanium, 0.3% niobium and 0.4 % carbon. The gun is possible to focus its electron beam on an extremely small spot of down to 20 nm in diameter. The emission current of the gun is 100μA and is stable over a period of 8 h. Standard stainless steels (NBS) were used for the preparation of calibration curves for chromium, iron and nickel. An identical, linear relation was obtained for the three elements between contents (mol % of the respective element) and intensity ratios. The ratios are those of the peak intensities of the respective element to the sum of the peak intensities of the three elements; chromium 489 eV, iron 651 eV, and nickel 848 eV. This technique was applied to analyze carbides in the casting steel. Two different carbides were found, and their compositions were estimated to be (Nb0.2Ti0.8)C and (Fe0.27Cr0.73)23C6, respectively.View full abstractDownload PDF (4924K) -
Minoru OKADA, Kenji OKAMURA, Hitoshi KIGAMI1980 Volume 29 Issue 6 Pages 356-360
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of aluminum in ferrovanadium using precipitation reaction of iron and vanadium with barium chloride was studied. Vanadium were precipitated by barium chloride in alkaline solution, and aluminum could be collected quantitatively at pH 12.513.0, ferric ion did not interfere with the determination. Vanadium reacted quantitatively with barium, in a mole ratio of V/Ba as 1/(1.41.6), to form Ba5Cl(VO4)3 or Ba3V2O8. The standard procedure is as follows : Transfer 0.500 g of the sample to a 250 ml beaker, and dissolve in 20 ml of H2O, 5 ml of HCl and 10 ml of HNO3. Dilute to 150 ml with hot water and heat until salts dissolve. Add 10 ml of 25 % BaCl2 solution and 25 ml of 50 % NaOH solution, stirring thoroughly. Boil a few minutes and transfer this solution to a 250 ml volumetric flask, cool to room temperature, and dilute to the mark. Filter through a fine paper, transfer 100 ml of filtrate to a 500 ml beaker and dilute to 250 ml. Adjust the pH to 1.0 with HCl and then to 3.0±0.1 with 20 % NH4Ac solution. Boil a few minutes and add 4 or 5 drops of Cu-PAN indicator solution. Titrate with EDTA solution until the color changes from wine red to yellow, and then add 1 or 2 ml in excess. Record the buret reading and boil a few minutes. Titrate the excess EDTA with CuSO4 solution to a wine red end point. This method is easy to remove iron and vanadium, and, in addition, highly accurate results can be obtained.View full abstractDownload PDF (829K) -
Tsutomu FUKASAWA, Masaaki IWATSUKI, Hiroshi KAWASAKI1980 Volume 29 Issue 6 Pages 360-366
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThis paper describes the weight- and phase-changes of sewage sludges, digested and undigested, when stored under air- and nitrogen-atmospheres of different humidities at room temperature. The growth of must was often observed when the sludges were kept standing under air, and Ca (OH)2 in the digested sludge was changed into CaCO3 (calcite and vaterite). Under a nitrogen atmosphere of about 50 % humidity, the sludges were dried to constant weights without growth of must and change of Ca (OH)2 into CaCO3. However, hystereses were observed in the weight humidity curves of the sludges under the nitrogen atmosphere, and the hysteresis was remarkable for the digested sludge : The weight of the sludge stored under the nitrogen atmosphere of a given humidity was dependent on the humidity of an atmosphere in which the sludge was previously kept. Calcium hydroxide in the sludge was changed into an amorphous substance in high-humidity atmosphere. The undigested sludge showed a weight decrease, which was not attributable to a decrease in water content. These sludges, if kept in a nitrogen atmosphere of 50 % humidity, allowed reproducible weighing for about a month.View full abstractDownload PDF (1431K) -
Taitiro FUJINAGA, Satoshi OKAZAKI, Toshitaka HORI1980 Volume 29 Issue 6 Pages 367-372
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA flow-coulometric method at the column electrode has been developed for the determination of orthophosphate ion. The principle of the method was as follows : Into a steady flow of carrier solution composed of 0.05 M Na2MoO4, 1.2 N H2SO4, and 20 % ethanol, was injected an aliquot of (10100)μl of phosphate sample. The phosphomolybdate complex formed instantaneously (within 20 s) in the flow line was led to the column electrode kept at +0.25 V vs. Ag-AgCl. The electrolytic reducticn proceeded with 2-electrons per molecule. The reduction current of the complex was recorded automatically and the amount of phosphate was determined from the net electricity consumed for the electrolysis. When an aliquot of 100 μl of sample injected at each run to the carrier stream controlled at a rate of 5 ml/min, the sample containing phosphate ranging from 1 ×10-5 M to 1 × 10-3 M can be analyzed within 2 min.View full abstractDownload PDF (909K) -
Motohisa FURUSAWA, Masaki TACHIBANA, Hiroshi KODAMA1980 Volume 29 Issue 6 Pages 372-376
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA liquid-liquid extraction procedure has been developed for separating carbazole from the related polynuclear aromatic compounds. Carbazole was first extracted from the cyclohexane solution into (8485) % sulfuric acid, and then back-extracted into fresh cyclohexane by diluting the sulfuric acid with water. After separation, the subsequent determination was carried out by spectrofluorometry. Carbazole in 20 ml of the sample solution was extracted into 10 ml of sulfuric acid at room temperature. On separating two layers, the sulfuric acid layer was separated from the cyclohexane and poured into 70 ml of water. The cyclohexane layer was washed with 5 ml of sulfuric acid and this sulfuric acid was combined with the preceding one. Then, carbazole was back-extracted into 10 ml of fresh cyclohexane. By this method, (0.580) μg of carbazole in (110) mg of the sample could be separated. The recovery was 97 % with 0.53 % of coefficient of variation. Carbazole could be determined by measuring the relative fluorescence intensity at 345 nm with excitation at 325 nm. As a standard, 1 μg/ml solution of carbazole was used. Incompleteness of the recovery was corrected by using the calibration curve obtained under the identical conditions as the sample. The method was not interfered by the presence of 10 mg of phenanthrene, fluorene, dibenzofuran, and biphenyl, 5 mg of acenaphthene, 1 mg of anthracene and fluoranthene, 0.5 mg of pyrene, 2 μg of anthraquinone and phenanthrenequinone, and 20 μg of 9-fluorenone.View full abstractDownload PDF (722K) -
Machiko TEZUKA, Michie NAKAYANAGI, Fujiko YAGYU, Shigeyuki TANAKA1980 Volume 29 Issue 6 Pages 376-381
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and simple method for classifying and characterizing crude oils by means of the combined infrared and proton nuclear magnetic resonance spectrometry has been investigated. From the infrared and nuclear magnetic resonance spectra of 60 crude petroleum samples, including the domestic, Middle East and others, absorbance of the band at 1600 cm-1, and the methylene to methyl proton intensity ratio, CH2/CH3, were measured respectively. The former can be considered to be related to the aromatic content, and the latter as having some relation to the structure of alkanes contained in crude petroleum. The values obtained from each crude oil were plotted on the log (I0/I) vs. CH2/CH3 two dimensional diagram. Standard deviations of the analyses were small enough to allow those values to be regarded as characteristic to each crude, petroleum. From the diagram, it was revealed that the domestic and Middle East crude oils formed distinct groups, not overlapping with each other. The plots of crude samples from the other areas were distributed widely on the diagram, indicating the presence of many different characteristics. This method is not only ureful for distinction of the domestic crude oils from the Middle East, but also applicable to correlation and identification of unknown petroleum samplesView full abstractDownload PDF (883K) -
Yoshimasa TANAKA, Yutaka SAITO, Junichi ODO, Hiromasa OMORI1980 Volume 29 Issue 6 Pages 381-384
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSilver ion shows a red color on the reaction with 4-hydroxybenzalrhodanine (HBR) in an alkaline solution. After elimination of disturbing ions such as mercury (II) and iron (III) by ammonia water, silver could be specifically detected. In the presence of diverse ions, the detection limit was measured. By using the same reaction, a spectrophotometric method for the determination of silver has been investigated. Five milliliter of a sample solution containing less than 16μg of silver ion was taken in a test tube and 3 ml of buffer solution (mixture of the same volume of 0.1 M sodium hydroxide and 0.1 M sodium citrate) and 2 ml of reagent solution (1.5 × 10-4 M HBR) were added. The absorbance of the mixture was measured at 490 nm against the reagent blank. Beer's law held for (216)μg of silver ion per 5 ml. The molar absorptivity and a coefficient of variation were 1.47 × 104 and 1.52 %, respectively. The presence of iron (III), cobalt (II) and mercury (II) caused an error. However, after elimination of these ions by ammonia water in the presence of iron (III), silver could be determined without disturbance.View full abstractDownload PDF (404K) -
Spectrophotometric determination of longchain aliphatic amines with chrome-azurol S-aluminum chelateYutaka SAITO, Jun TANAKA, Junichi ODO, Yoshimasa TANAKA1980 Volume 29 Issue 6 Pages 385-389
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe precipitation of ternary complex of chromeazurol S, Al (III) and long-chain aliphatic amine was avoided by adding 20 % ethanol, and the solution was submitted to a spectrophotometric determination of the amines. The reagent solution was fixed as 3 : 2 mixture of 1.0 × 10-4 M chrome-azurol S in ethanol and 1.5 × 10-4 M aluminum potassium sulfate in pH 4.8 Walpole buffer, and 5 ml reagent solution was added into 10 ml sample solution. After standing for 20 min, the absorbance was measured at 640 nm against a reagent blank. In the case of octadecylamine (ODA), Bee's low held from 2.5 to 10.0 μg/ml, the ε value and coefficient of variation being 1.85 × 1041 mo1-1 cm-1 and 0.86 % for 10 μg/ml, respectively. This method was applied to n-butyl-n-octadecylamine, diethyl-n-hexadecylamine and cetyltrimethylammoniurn salt etc. Several ions such as F-, Fe(CN)63- and Hg2+ interfere the determination. In order to avoid the interference, acetic acid (1 ml) was added to the -ample solution, and ODA was extracted with chloroform. After removing chloroform in vacuo, the residue was dissolved in 10 ml water, and ODA was determined by this method. The determination of ODA was not interfered by the presence of 500-fold of the ions.View full abstractDownload PDF (794K) -
Spectral interference in atomic absorption spectrometry. VIHidehiro DAIDOJI1980 Volume 29 Issue 6 Pages 389-395
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMolecular absorption obtained by gallium solutions containing hydrochloric acid and nitric acid in airacetylene and argon-air-hydrogen flames were measured in the wavelength range 200 nm to 420 nm. Atomic absorption spectrophotometer Hitachi 207 was used with Hamamatsu TV D2 lamp and some hollow cathode lamps. Absorption spectra in two flames were detected band of GaCl in (245260) nm region and unknown band in (200310) nm region. The band in (200310) nm region was presumed to be due GaOH. The absorbances on these bands were in proportion to the gallium concentration. Thus, these molecular absorptions were interfered in atomic absorption spectrometry when the sample solution was containing high concentration of gallium salts. Especially, the interference at iron resonance line of 248.3 nm was greatest. On the other side, the ratios of the concentrations of GaOH (CGaOH) GaCl (CGaCl) and Ga (CGa) to total concentrations of gallium (CT) in the flame can be obtained by absorbances on these spectra as previously reported. Here, CT = CGa + CGaOH+CGaCl. The absorbances were measured at 294.3 nm of atomic line of gallium, 241 nm of GaOH and 249 nm of GaCl molecule bands at various positions in argon-air-hydrogen flames as a function of hydrogen flow rate. At 15 mm height above burner head in rich hydrogen flame, the values of CGa/CT (= β), CGaOH/CT and CGaCl/CT for the solution containing hydrochloric acid were obtained as 0.51, 0.41 and 0.09, respectively. And the β values for the solution containing nitric acid was 0.55.View full abstractDownload PDF (618K) -
Daijiro YAMAMOTO, Masamichi TSUKADA, Shozaburoh HIRAOKA1980 Volume 29 Issue 6 Pages 396-399
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDiammonium ethylene-bis-dithiocarbamate (DETC) reacts with nickel (II) and forms a water-insoluble greenish brown complex in aqueous solution at pH 6.5, which can be extracted with MIBK containing 1 v/v % TBP. The extraction-spectrophotometric method for the determination of nickel (II) based on this reaction was studied. The recommended procedure is as follows : To a sample solution (4 cm3) containing (0.26.0) μg, was added 8 cm3 of Britton and Robinson buffer (pH 6.5), and the mixture was heated for 10 min at 50°C. The resultant solution was mixed with 2 cm3 of 0.5 % DETC aqueous solution and heated for 25 min at 50°C. After cooling for 3 min in ice-water, nickel (II) in the solution was extracted with 4 cm3 of MIBK containing 1 v/v% TBP by shaking for 2.5 min. The absorbance of the extract was measured at 385 nm against the reagent blank. The apparent molar absorption coefficient of the complex was 3.65 × 104 dm3 mol -1 cm-1, and the Beer's law obeyed the concentration range from 0.05 to 1.50 μg cm-3 of nickel (II). The molar ratio of nickel (II) to DETC in the complex was estimated to be 1 : 2 by the continuous variation method. Various metal ions, such as cobalt (II), copper (II), iron (II) and (III), lead (II), molybdenum (VI), palladium (II), strontium (II), zinc (II), interfered. These interfering metal ions could be removed by extraction of nickel (II) as dimethylglyoximate complex with chloroform.View full abstractDownload PDF (448K) -
Mitsuhiko TAGA, Shunitz TANAKA, Hitoshi YOSHIDA1980 Volume 29 Issue 6 Pages 400-405
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe peak of copper by differential pulse anodic stripping voltammetry was enhanced by the addition of iodide ion. Copper was deposited on the hanging mercury drop electrode (HMDE) for 5 min at -0.5 V vs. SCE and stripped in 0.1 mol dm-3 acetate buffer solution (pH 4.5) containing 2.5 × 10-5 mol dm-3 iodide ion. The peak current increased about 4 times as large as that in the solution without iodide ion. The stripping peak current was largely influenced by the scan rate. The maximum peak current was observed at 2 mV s-1, and when the scan rate became faster than 2 mV s-1, the peak current decreased. The peak current was proportional to the concentration of copper over the range of (5 × 10-87 × 10-7) mol dm-3. The relative standard deviation for 5 runs at 1 × 10-7 mol dm-3 Cu (II) was ca. 3 % and the lower detection limit was 0.2 ppb under the deposition time of 10 min. This method also facilitated the determination of copper in the presence of chloride ion. When copper was stripped in the solution containing 1 × 10-2 mol dm-3 chloride ion, the peak of copper was obscured and the relation between the peak current and the concentration of copper became non-linear. But by the addition of iodide ion the peak current was increased, and the linearity was restored. The effects of other co-existing ions were studied.View full abstractDownload PDF (1013K) -
Junko HARA, Nobuo SUZUKI, Koichi SAITOH1980 Volume 29 Issue 6 Pages 405-409
Published: June 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe liquid chromatographic behavior of eight β-diketones were made in the column systems of an OPN-chemically bonded stationary phase (Durapak OPN/Porasil) and various mobile phase solvent, viz., toluene, chlorobenzene, benzene, 1, 2-dichloroethane, ethylbenzene, ethylacetate, and 2-methyl-4-pentanone. The β-diketones investigated were acetylacetone (A), benzoylacetone (B), 3-phenylacetylacetone (C), dibenzoylmethane (D), furoyltrifluoroacetone (E), trifluoroacetylacetone (F), thenoyltrifluoroacetone (G) and benzoyltrifluoroacetone (H). The results are summarized as follows: (1) The sequence of retention volume for these β-diketones does not give a consistent order in different mobile phase systems. However, when these compounds are classified into two groups with regard to the presence of functional group -CF3 in molecule, the retention order of D<C<B<A and H<G<F<E are regularly observed in every solvent system; (2) the retention of a β-diketone decreases with an increase in the solvent strength, ε°, of the mobile phase used; and (3) the retention behavior of the compounds on the OPN-bonded silica gel is apparently similar to those on a simple silica gel.View full abstractDownload PDF (606K) -
Shigeru FUKUSHIMA, Hidenari INOUE, Tsuneo SHIRAI, Saburo YANAGISAWA1980 Volume 29 Issue 6 Pages 410-412
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new method was proposed for the determination of nitrogen oxides in flue gases. A volume of 50 ml each of sample gases was introduced into a 100 ml syringe, followed by the addition of 20 ml of the alkaline absorption solution containing 0.03 % hydrogen peroxide and 30 ml of oxygen. After the completion of the (1520) min oxidation and absorption of nitrogen oxides, one ml of 6 N sulfuric acid was added to the absorption solution in order to decompose the excess of hydrogen peroxide by the careful addition of a 0.3 % solution of potassium permanganate. The pH range of the obtained solution was adjusted to 68 and the nitrate ions determined by the same analytical procedure as that of the zinc reductionnaphthylethylenediamine method. With the present method nitric oxide of about 85 ppm was successfully determined without any interferences of ammonia of up to 1000 ppm and of sulfur dioxide of more than 1000 ppm.View full abstractDownload PDF (437K) -
Itsuo MORI, Yoshikazu FUJITA, Kimiko SAKAGUCHI, Takehisa ENOKI1980 Volume 29 Issue 6 Pages 413-416
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA highly sensitive method has been developed for the spectrophotometric determination of molybdenum(VI) with gallein and hydrogen peroxide in a neutral aqueous solution. The calibration curve for the spectrophotometric determination was linear in the range of (0.010.2) μg molybdenum(VI)/10 ml. The sensitivity was 0.00003 μg molybdenum(VI)/cm2 for absorbance of 0.001. The recovery of molybdenum(VI) in a waste water is (97.5102.0)%. The recommended analytical procedure is as follows. A sample solution containing less than 0.2 μg of molybdenum(VI) is taken in a 10 ml measuring flask. Two ml of 1.0 % polyvinylalcohol solution, 1.0 ml of 3.0 % hydrogen peroxide solution and 0.75 ml of 1.0 × 10-3 M gallein methanol solution are added, and then the resulting solution is adjusted to pH 6.46.9 with phosphate buffer solution. The volume is made to 10.0 ml with redistilled water, and the solution is kept at 60°C for 90 min and cooled for 5 min in water. Within 15 min the difference in absorbance between, gallein-hydrogen peroxide solution and gallein-hydrogen peroxide-molybdenum(VI) solution is measured at 530 nm against water. The effect of diverse ion on the determination of molybdenum(VI) was examined. Thorium(IV), copper(II), nickel(II), iron(III) and chromium(VI) etc. interfered, but thorium(IV), nickel(II), copper(II) and zinc(II) could be masked by the addition of 0.1 M nitrilotriacetic acid solution.View full abstractDownload PDF (660K) -
Kensaku HARAGUCHI, Masahiro MIYAJIMA, Saburo ITO1980 Volume 29 Issue 6 Pages 416-418
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS2-(2-Pyridylazo)-5-methylphenol (PAP-5-Me) was synthesized, and its acid dissociation constants and the color reaction with metal ions were determined spectrophotometrically. PAP-5-Me is prepared from 2-hydrazinopyridine and 4-methyl-1, 2-benzoquinone with a yield of (6067)%. The product, red-colored needle-like crystalline solid melting at (100101)°C, is soluble in organic solvents such as alcohols and chloroform and also to a slight extent in water. The acid dissociation constants of the reagent are pKa1=2.55±0.02 and pKa2=8.75±0.02 at 25°C and μ=0.1. PAP-5-Me forms water-insoluble chelates with a large variety of metal ions. These chelates are made water-soluble by nonionic surfactant, Triton X-100. The color reaction of the reagent with metal ions shows that it will be applicable for the spectrophotometric reagent of metal ions.View full abstractDownload PDF (454K) -
Toshiaki FUJII1980 Volume 29 Issue 6 Pages 418-420
Published: June 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe formula of composting municipal refuse and sewage sludge is given the attention of the public in recent years. However, the marker of determination of ripeness was yet unknown and determination was been based on experience. Author studied the change of water soluble substances in fermenting compost by gel permeation chromatography (GPC). The results as follows. (1) The changes of substances in compost easily can be detected by GPC. (2) Changes of molecules from 10 to 5000 and from 5000 to 100000 reveal the processes of first and the second fermentation, respectively.View full abstractDownload PDF (474K)
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