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Volume 27, Issue 2
Displaying 1-16 of 16 articles from this issue
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Kazuo SETA, Mitsunori WASHITAKE, Toshio ANMO, Nobuharu TAKAI, Tsuneo O ...1978 Volume 27 Issue 2 Pages 73-77
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSeveral high-resolution anion-exchange chromatographic systems using microreticular anion-exchange resin have been developed for the analysis of various physiological fluids. However, these liquid chromatographic: systems require a relatively long separation time {measured in (2040)h}, resulting in a low sample throughput rate. In this paper, a high-speed and high-resolution liquid chromatographic method which separates about a houndred ultra-violet-absorbing constituents of human urine in less than 120 minutes was studied; i.e. a 100-μl urine sample was chromatographed on a 0.4×50 cm column packed with strongly basic macroreticular anion-exchange resin (5 to 7μm-diameter CDR-10, Mitsubishi Chemical Industries, Ltd., Tokyo, Japan) derived from styren-divinylbenzene type porous polymer having 35 % cross linkage, and eluted with a linear acetate (pH 4.4) gradient from 0.006 to 6.0 M at an average flow-rate of 0.71 ml/min and an average pressure of 105 kg/cm2. The reproducibility of retention times and peak heights in this system has been demonstrated to be better than ±2% as relative standard deviation. In addition, the effects of the flow-rate and the pH of acetate buffers on the separation, and the property of the resin were investigated. In conclusion, a short column containing small, macroreticular anion-exchange resin beads has been shown to produce a more rapid separation of the constituents of physiological fluids than that obtained with relatively long column of microreticular anion-exchange resin beads.View full abstractDownload PDF (761K) -
Hiroshi NISHIDA1978 Volume 27 Issue 2 Pages 77-81
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBeryllium forms a complex with Chromazurol S (CAS) in a 1 : 2 molar ratio in the presence of polyoxyethylenedodecylamine (POEDA). The absorption maximum of the complex is at 605 nm and its molar absorptivity is 1 ×105 1 mol-1 cm-1. In an equilibrium state, the absorbance of the complex does not depend on the kind of anions contained in the sample solution. In addition, the kinetics have been investigated for this complexation reaction. The reaction is of the pseudo first and second with respect to the concentration of beryllium on and CAS, respectively, and independent of a hydrogen ion concentration over the pH range from 4.4 to 5. The rate of the complexation reaction decreases slightly with an increase in the concentration of POEDA. The reaction rate increases with increasing the concentration of anions and in the same anion concentration it increases in an order of EDTA>>perchlorate>nitrate>chloride≥sulfate. On the basis of these results, the rate-determining step of this reaction may be the reaction between beryllium ion and GAS ion in the vicinity of the charged micelle surface formed from POEDA. The addition of EDTA is most effective for acceleration of the reaction rate, but an excess of EDTA (above 0.025 M) interfers with the complex formation.View full abstractDownload PDF (758K) -
Eiko AMAKAWA, Kazuo OHNISHI, Nobuo TAGUCHI, Hiromaro SEKI1978 Volume 27 Issue 2 Pages 81-84
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTin was determined by flameless atomic absorption. spectroscopy. Interferences of diverse ions were removed by mean of coprecipitation with zirconium hydroxide and simplified standard addition method. Sample, 2 to 5 g, was ashed by wet method with nitric-perchloric acid. After addition of 1 drop of phenolphthalein solution and 1 ml of 3.5% zirconium oxichloride solution, the sample solution was added 28% ammonia water dropwise with strring slowly until the solution turned red. The precipitate was filtered through Toyo No. 5A filter paper and washed with distilled water. The residue was dissolved in 30 ml of hot 5% hydrochloric acid. Tin was determined by simplified standard addition method; after the sample solution and standard solution was separately injected in the graphite tube, those were atomized at the same time. Tin was coprecipitated with zirconium hydroxide at pH 5 to 9. As3+, Na+, K+, Ca2+, and Mg2+ did not coprecipitate with zirconium hydroxide, 10000 times of those had no effect on the determination of tin. In the simplified standard addition method, 100 times of Al3+, Fe3+, Zn2+, Cu2+, Pb2+, Ni2+, Cd2+ and As3+ coprecipitated with zirconium hydroxide, did not interfere with the determination of tin. But 500 times (10 mg) or more of phosphate ion decreased the recoveries of tin. This method was applied to the determination of tin in soft drinks. The recoveries of tin were 100 to 106% and the coefficient of the variation was 2.3%.View full abstractDownload PDF (582K) -
Takanori AKIYOSHI, Takako TSUKAMOTO1978 Volume 27 Issue 2 Pages 85-89
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTrace amount of boron in steel were determined by means of emission spectrometry using high frequency plasma torch. The sensitivity of this method depended on the kind of solvent used, and methyl alcohol gave the best sensitivity. The determination limit of boron in methanol was 0.002μg/ml. The established method utilized the high sensibility of the plasma torch and the easy distillation of boron in methanol as trimethylborate {B(OCH3)3}. The sample was dissolved by acids and dehydrated by hot H2SO4 and H3PO4. After cooling and addition of methanol (60 ml), the solution was distilled to obtain 40 ml of the distillate. The amount of boron in the distillate was determined by the intensity of the spectral line of B 2497. 73 Å excited by plasma torch. This method was rapid and accurate, particularly in determining trace amounts of boron and the determination range of boron in steel was 0.2 to 150 ppm. This method was also appliciable to stainless steels and other alloys.View full abstractDownload PDF (717K) -
Tsutomu FUKASAWA, Masaaki IWATSUKI, Susumu KAWAKUBO1978 Volume 27 Issue 2 Pages 90-95
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe powder X-ray diffraction analysis become often difficult by preferred orientation on the sample holder of the crystallites of the component to be analyzed. In this paper, the preparation of an orientation-free specimen for the sample of less than a few milligrams is described. Orthorhombic lead(II) oxide powder, easily exhibiting preferred orientation by the conventional sample mounting, was used for this study in the forms of oxide alone or its mixture with magnesium oxide. By use of a sample scattering device designed, the sample was scattered onto an adhesive tape coated with particulate matters, adhesive cloths or others, which was previously sticked on the conventional aluminum holder, etc. The relative intensities of representative diffraction lines 111 and 002, which show the largest orientation-effect, and others were measured to estimate an orientation index defined by authors and precision of intensity measurements. An orientationfree specimen was prepared by use of an adhesive tape coated with glass granules coarser than 150 mesh or globular ion-exchange resin of (150200) mesh, or nylon-cloth for stockings coated with an adhesive. The relative standard deviation of the relative intensity was about 12% for 002 line according to the way described above. The conventional ways were also tried by use of the same sample, and compared with the ways developed here.View full abstractDownload PDF (1186K) -
Kazuhiko TANAKA, Hiroshi SUNAHARA1978 Volume 27 Issue 2 Pages 95-99
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the separation and indirect detection of phosphate, phosphite and hypophosphite in a mixture by ion exclusion chromatography with a hydrogen-form cation exchange resin, a flow coulometric method was used for the detection of hydrogen ion liberated by cation-exchange. The chromatographic conditions such as the composition of an eluent containing organic solvents and column temperature were investigated. For a water eluent, the capacity factor (k') of these anions were 0.051 for phosphate ion, 0.018 for phosphite ion and 0.038 for hypophosphite ion, respectively, and depended on the first dissociation constant (pK1) of the corresponding acid. For the eluent of water-organic solvents or water-perchloric acid, the k' of these anions increased with decreasing dielectric constant of the eluent caused by the addition of organic solvents, such as methanol, ethanol and acetone. The increase of k' occurred also by the addition of perchloric acid. For the water-acetone eluent, the logarithm of k' of these anions increased linearly with the increase in the acetone concentration from 0 to 80%(v/v) and the increase in column temperature from 25 to 80°C. Each electrolytic efficiency of these anions obtained from the chromatogram peak area decreased with increasing acetone concentration, being 90% for hypophosphite ion, 57% for phosphite ion and 50% for phosphate ion, respectively, under the conditions of the 80%(v/v) acetone and flow rate of 1 ml/min. The separation of a mixture of these anions can be best achieved by elution with 70% (v/v) acetone at 50 °C.View full abstractDownload PDF (769K) -
Shigeko NAKAZAWA, Kunio TANAKA1978 Volume 27 Issue 2 Pages 100-104
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSHalides and hydrohalogenides of organic bases were titrated potentiometrically with perchloric acid in glacial acetic acid-dioxane solution after the addition of bismuth nitrate in place of mercury(II) acetate in order to remove the effect of halide. The new method proposed was as follows: Weigh accurately about 0.7 × 10-3 equivalence of the sample, previously dried, dissolve in 40 ml of glacial acetic acid, add 40 ml of dioxane and 2.5 ml of 5% bismuth nitrate in glacial acetic acid, and titrate with 0.1 N perchloric acid potentiometrically. Perform a blank run in the same manner and make any necessary correction. The coefficient of variation of this method was found to be 0.18% in fifteen runs. The effect of bismuth nitrate on the change of potential at the equivalence point was examined. The mole ratio of Bi/Halogen=0.350.42 (equivalence ratio of Bi/Halogen =1.051.26) was suit-able for the determination. The proposed method was successfully applied to the determination of various compounds, and also may be used satisfactorily for practical rutine analysis.View full abstractDownload PDF (829K) -
Toshiyuki HOBO, Yoshihisa SUDO, Shigetaka SUZUKI, Shun ARAKI1978 Volume 27 Issue 2 Pages 104-108
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe foam separation technique developed for the concentration of methyl mercuric chloride in water has been applied to the concentration of Cu(II) ions. A system shown in Figs. 1 and 2 was newly devised. Initially, the batch type experiments were conducted for 1000 ml samples and the following procedure was found to be appropriate: Adjust the sample pH at 9.0 and add 40 ml of 0.5% potassium n-butyl xanthate (n-BuXn) solution. Then, under the nitrogen gas flow rate at 500 ml/min and 0.075% cetyltrimethylammonium bromide (CTAB) solution supply rate at 90 ml/h, collect the foam comes out of the separator for 40 min. The concentration ratio of 100 and almost 100% recovery of Cu(II) ions from 2 x 10-8 g/ml solutions were achieved through above procedure. The continuous separations were also examined at sample solution flow rates of 1000, 2000 and 4000 ml/h. A satisfactory result was obtained from the 1000 ml/h experiment. The other conditions in the experiment were as follows: pH; 9.0, n-BuXn solution supply rate; 66 ml/h, CTAB solution supply rate; 111 ml/h, nitrogen flow rate; 1000 ml/min. The foam subsided in every 30 min in the receiver which contained 0.1 ml of n-butanol was measured of its Cu(II) ion content by using atomic absorption spectrometry. In this case, recovery was about 96% and concentration ratio was about 50. By connecting a continuous detector such as a photometric one a good pollution monitor system will be realized.View full abstractDownload PDF (749K) -
Fluorometric determination of aluminum in sea waterKiyotoshi MORISIGE, Keizo HIRAKI, Yasuharu NISHIKAWA, Tsunenobu SHIGEM ...1978 Volume 27 Issue 2 Pages 109-114
Published: February 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSEleven Schiff bases, which are derived from salicylaldehyde-semicarbazone, were synthesized, and the effect of the position of substituent groups on the fluorescence properties of metal complexes was studied. The compounds of these types formed the fluorescent complexes with aluminum, gallium, scandium, yttrium and zinc ions. In generally, substitution by o, p-orientating substituents at p-position to -CH=N- group of Schiff bases and substitution by m-orientating substituents at m-position increased fluorescence sensitivity index (F.S.I.) and molar extinction coefficient of the complexes. These values correlated with Hammett's substituent constant. The phenomenon may be explained by the concept of charged quinoid form, and significant contribution of charged quinoid form enhanced the fluorescence ability of the complexes. 2, 4-Dihydroxybenzaldehyde-semicarbazone proved a good fluorescence reagent for aluminum determination, on account of the stability and sensitivity of fluorescence, and then, this reagent was used for the rapid and accurate determination of aluminum in sea water. An analytical procedure for the determination of aluminum in sea, water is as follows: To (510) ml sample solution containing an appropriate amount of aluminum ion, 2 ml of a 0.1% 2, 4-dihydroxybenzaldehyde-semicarbazone solution and 2 ml of 20% ammonium acetate are added. The pH of the solution in adjusted to 5.5 with diluted hydrochloric acid or ammonia, and the solution is diluted to 25 ml with water. The fluorescence intensity of the solution is measured (λ excitation 353 nm, λ emission 413 nm). In this procedure, relative standard deviation was 0.080±0.005 μg for sea water (sea water sample: 10 ml).View full abstractDownload PDF (908K) -
Kunishige HIGASHI, Kazuyoshi HAGIWARA1978 Volume 27 Issue 2 Pages 115-120
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt is important to develop an analytical method to clarify the source of oil spill. The discrimination of petroleum oils was studied by gel permeation chromatography (GPC) with ultra-violet spectrometric detector. Petroleum oil sample was diluted with tetrahydrofuran and 12μl of the sample solution was analysed with a high speed liquid chromatography. A column (50 cm in length and 7.9 mm in internal diameter) packed with HSG-15 (Polystylene gel, Shimadzu) was used at 50°C. Tetrahydrofuran was used as an eluent under 50 kg/cm2 pressure. Chromatogram was recorded by measuring absorbancy of the eluate with ultra-violet spectrometric detector. The detection wavelength was fixed in the range of 240 nm to 400 nm. The influence of the detection wavelength on a profile of a chromatogram was studied on eight kinds of crude oils (Minas, Murban, Khafji, Iranian light, Oman, Kuwait, Hout, Iranian heavy) and petroleum products (kerosene, gas oil, lubricating oils and fuel oils A, B and C). The profile of the chromatogram changed considerably with the detection wavelength in the range of larger retention time for the crude oils and the fuel oils. A practical procedure of the discrimination of the oils was proposed as follows. The oils can be classified in to two groups by measuring the chromatogram at 254 nm. Group 1; kerosene, gas oil, lubricating oils, fuel oil A; Each product can be discriminated measuring the retention time by GPC or gas chromatography. Group 2; fuel oils B, C and crude oils; The discrimination among Minas, Murban and Khafji crude oils, fuel oil C and the discrimination of these oils from the Group 1 are easy. The discrimination capability of the crude oils which have similar profiles at 254 nm can be improved by the measurement of the chromatogram at 280 nm.View full abstractDownload PDF (651K) -
Kunio NAKANO, Takemi MIURA1978 Volume 27 Issue 2 Pages 121-123
Published: February 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe determination of copper in a very diluted solutions which could not be detected by the ordinary carbon tube method became possible by a multifold concentration method. The method is carried out by atomizing after repeated injection of sample and drying. However since the reproducibility tends to decrease when the conventional carbon tube (type A) is used, an attempt was made to improve the carbon tube. The first one (type B) has a smaller injection window of 1.5 mm diameter, so as to stopper the top of the pipette at fixed position. The second one (type C) has a small hole right under the injection window of type B. The reproducibility was improved by using the new tubes but type C was better than type B when the number of times of injection repeated was increased. Although the relation between the peak height and the number of times repeated was linear within fifteen times, the peak height slightly exceeded the expected value over twentytimes.View full abstractDownload PDF (457K) -
Yoshihisa TANABE, Junko MIYATANI1978 Volume 27 Issue 2 Pages 123-125
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid method for the microdetermination of nitrogen in cyanides, cyanocomplexes and apricot kernel water is proposed. The method is based on the reductive decomposition of cyano group to the mixture of ammonia and methylamine in alkaline medium by using Raney nickel and subsequently on the titration of the mixed bases which are distilled and collected in 4% boric acid, using 0.01 N HC1 as titrant. The reduction and the distillation were carried out with the improved micro Kjeldahl apparatus previously reported by the author. A (510) mg of sample was taken in the distillation flask, and the appropriate quantity of Raney nickel powder (0.35 g for ordinary cyanides, 0.45 g for cyanocomplexes) was added, the powder then being washed down with (510) ml of water. After the whole apparatus was assembled by glass joint, 2 ml of alkaline solution (30% NaOH) and 5 ml of water were run in through the introductory funnel and the condenser tip was put beneath the solution of boric acid in the receiver. The distillation flask was heated gradually by a burner flame under aeration (one or two bubbles per second) till red colored boric acid solution with methylred turned to pale yellow. After the violent distillation for fifteen minutes, the microtitration with 0.01 N HCl was carried out in that the blank value was suggested to be substracted from the experimental value. The standard deviation and the coefficient of variation were (0.20.1)% and (1.10.5)%, respectively, in a series of experiments. NO3-, NO2-, SCN-, CNO-, NH4+ and volatile amines interfere the analysis.View full abstractDownload PDF (617K) -
Kenji YAMAGUCHI, Itsuo OKUMURA, Masakazu DEGUCHI1978 Volume 27 Issue 2 Pages 125-128
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCadmium was quantitatively extracted by shaking thiothenoyl-trifluoroacetone (STTA) solution in xylene in the presence of ο-phenanthroline from an aqueous solution at pH 4.09.0. The resulting organic phase directly subjected to atomic absorption spectrophotometry. The determination of small amounts of cadmium in tin metal by use of this analytical technique was investigated. A required amount of the sample (0.5 g) was dissolved by heating in 5 ml of nitric acid (1+1), and was evaporated to (23) ml on a hot plate. The residue was dissolved in 150 ml of warm water and filter pulp was added. The solution containing the precipitate was stood for 30 minutes on the hot plate. The solution was filtered through filter paper, and the residue was washed with warm water. After the pH of the filtrate was adjusted to 5 by adding acetate buffer (pH 5.0) and ammonium hydroxide (1+10), the solution was taken into a separatory funnel. Five milliliters of 1.5 × 10-3 M ο-phenanthroline solution and 10 ml of 8.4 × 10-4 M STTA solution in xylene were added. After shaking for 3 minutes, the organic phase was introduced into air-acetylene flame and the absorbance was measured at 228.8 nm. The calibration curve was linear for 010μg of cadmium in 10 ml of the organic phase, and the coefficient of variation was within 2.7%. The sensitivity was 0.017 μg/ml [xylene]/1%. No appreciable interference was caused by other impurities likely to be present in tin metal. The accuracy of the procedure was checked by B.A.M. standard samples with good agreement. The proposed method was successfully applied to the determination of cadmium above 0.0002% in tin metal.View full abstractDownload PDF (712K) -
Toshio YAMASHITA, Toshio SASAKI, Mitsuru FUJIMURA, Yoshikazu HASHIMOTO1978 Volume 27 Issue 2 Pages T1-T5
Published: February 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAdsorption of sulfur dioxide and nitrogen oxides on glass fiber filters was found to be responsible for their weight increments in aerosol collection routine. Filters of eleven kinds were tested and the increments were correlated with the alkalinity of water extracts of the filters, which was in the order: GB 100, GB 100R (Toyo)>AE (Gelman)>GF/ F (Whatman)>CT 75428 (MSA)>GF/B, GF/C, GF/A, GF/D(Whatman)>type A (Gelman)>AP 20(Millipore). The alkalinity sequence of the filters (water extracts) was actually in accord with the sequence of their weight increments measured for aerosol-free atmospheric air, which was prepared by allowing the air to be passed through a quartz fiber filter. When the filters were exposed to sulfur dioxide (2000 ppm) or nitrogen dioxide {(11 000)ppm} in a closed vessel, the sequence of magnitude of gas adsorption on the filters was found to be similar to that found. in fields for aerosol-free air. Based on these observations we came to a conclusion that the filters of high alkalinity (water extracts) take up a considerable amount of sulfur dioxide in the atmosphere during air sampling, so that the gas adsorption effect should not be overlooked for measurements of atmospheric aerosols by glass fiber filtration technique.View full abstractDownload PDF (857K) -
Kichinosuke HIROKAWA, Masaoki OKU1978 Volume 27 Issue 2 Pages T5-T8
Published: February 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSemiquantitative analytical application of X-ray photoelectron spectroscopy has been investigated. The estimation of a layer composition under surface as well as a surface layer composition is described for nickel-copper alloys. The possible utilities of the X-ray photoelectron technique to the study of precipitation phenomena are also explored, which include the coprecipitation of lead sulfate with barium sulfate and the post precipitation of zinc sulfide on the surface of copper sulfide.View full abstractDownload PDF (595K) -
Kazuhisa ABE, Tokuko WATANABE, Shizuo FUJIWARA1978 Volume 27 Issue 2 Pages T9-T13
Published: February 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSOptimal conditions for the determination of nitroxide radicals by ESR were investigated with respect to several factors such as the power of microwave, the width of modulation, the sweep rate of magnetic field, and the time constant of spectrometer response. Result presented here are perhaps helpful to analysts working on the nitroxide radicals which have currently used in many fields of biological and medical interest.View full abstractDownload PDF (688K)
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