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Volume 42, Issue 4
Displaying 1-12 of 12 articles from this issue
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Teiichiro OGAWA1993 Volume 42 Issue 4 Pages 201-207
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA highly sensitive detection of photoabsorbing molecules can be carried out by the laser multi-photon ionization method combined with the conductivity measurement. Photoionization mechanism has been investigated by irradiating a laser beam on photoabsorbing molecules in solution and on surface. The photoionization current is due to the motions of electrons, cations and anions, and their time profiles are subject to a space charge effect. The analytical procedure has been optimized on the basis of the investigations on mechanism. Typical detection limits are the following: pyrene in hydrocarbon solvents was 6 ppt, pyrene in water was 9 ppt, and BBQ on a platinum surface was below 1% of monolayer coverage. This method can be applied to a highly sensitive HPLC detector. These results indicate that the laser multi-photon ionization is a sensitive and useful analytical technique.View full abstractDownload PDF (994K) -
Hatsuo SUGITANI, Yasuko NAKAMURA, Kouji ISOGAI1993 Volume 42 Issue 4 Pages 209-214
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe structure analysis of polyamic acid prepared from pyromellitic dianhydride (PMDA) and 4, 4'-diaminodiphenyl ether (DDE) was studied by 13C-NMR. The 13C-NMR signals of model compounds prepared from PMDA and aniline were assiglmed by 2D-NMR such as C-H cosy and coloc, followed the assignments of 13C-NMR signal of the amic acid oligomer prepared from PMDA and DDE. The 13C-NMR signals of polyamic acid were assigned by the application of the 13C-NMR signal assignments of model compounds and amic acid oligomer, and the structures of polyamic acid such as the meta/para ratio of amide bonds. The average length and the end-group of molecular chains were clarified.View full abstractDownload PDF (681K) -
Etsuko NAGATA, Shuuichi YASUDA, Tomoyuki KASAHARA, Hiroaki KUBO, Sadan ...1993 Volume 42 Issue 4 Pages 215-218
Published: April 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple, rapid and reproducible method for the determination of iodoform in rabbit plasma by HPLC has been developed. Under the light-resistant condition, iodoform and diiodomethane (as internal standard) in 1.0 ml plasma were extracted with 1.0 ml diethylether. Twenty microliters of the organic phase were injected into the HPLC system, consisted of a Model 510, U6K-injector, Model 481 UV detector setting at 336 nm (0.005 AUFS), an Ultrasphere ODS 5 μm guard column (45 mm × 4.6 mm i.d. ) and an analytical column (150 mm ×4.6 mm i.d.). The mobile phase was 60% methanol / pH 3.8, 5 mM potassium phosphate buffer. The flow rate was 1.0 ml/min. The retention time for iodoform and diiodomethane were 10.4 and 7.7 min, respectively. The limit of detection was 0.3 μg/ml (S/N=3) of plasma. Within-run reproducibility for 0.4 μg/ml was ± 2.1% (n=9). The HPLC separation can be completed in less than 11 min and had been applied for plasma of rabbit packed intraperitoneally by iodoform gauze.View full abstractDownload PDF (459K) -
Masayoshi KIYOKAWA, Hitoshi YAMAGUCHI, Ryosuke HASEGAWA1993 Volume 42 Issue 4 Pages 219-222
Published: April 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA modified fluoride separation-molybdosilicic acid blue spectrophotometry using masking reagent of iron was applied to determine trace silicon in high purity iron samples. The analytical procedure used is as follows; decompose 1.0 g of sample with a solution of sulfuric acid 2 ml and nitric acid 0.5 ml. After cooling the solution, add phosphoric acid 5 ml as masking reagent and hydrofluoric acid (1 %) 0.5 ml and then sulfuric acid 20 ml, to yield volatile silicon tetrafluoride. Transfer the fluoride completely into a boric acid solution by purging it with nitrogen. Then, move the solution into a 25 ml flask, and add hydrocloric acid and ammonium molybdate to form molybdosilicate. After adding oxalic acid and Ascorbic acid, measure the light absorbance of the solution at 810 nm. By this method, ppm level silicon in commercial high purity irons (4N and 5N) and subppm level silicon in JSS standard high purity iron sample were successfully determined. Recovery (n=10) was 96% for 10μg of silicon and the detection limit givcn by 3σ of blank value was 0.06 ppm.View full abstractDownload PDF (559K) -
Tetsuya KIRIYANIA1993 Volume 42 Issue 4 Pages 223-228
Published: April 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA preconcentration-spectrophotometric determination of copper in sea and fresh water samples is described. After the sample is treated with permanganate, copper is allowed to enrich on a strongly basic anion-exchange column (Amberlite CG 400 in the chloride form; φ1.0×4.5 cm) from 2l of acidified, heatcd sample water (40°C, 0.01 M in HCl) in the prescnce of 0.01 M ascorbic acid. To enhance the adsorption the fresh water is made saline before sorption by adding sodium chloride to yield ca. 0.5M concentration. Copper sorbed on the column can be stripped by elution wlth 20ml of 1 M nitric acid. Copper is then determined spectrophotometrically with diethyldithiocarbamate. This combined method is sensitive to as low as 2×10-10M of copper in 2l sample. Cadmium, nickel, manganese(II), lead, zinc, iron(III), cobalt, mercury(II)alld silver do not interfere in the presence of even 100 times as much as their contents in seawater samples. The precision (rsd) of 37% at a copper level of 0.40.8μg/l can be obtained.View full abstractDownload PDF (774K) -
Hiroki YONEZAWA, Koji SHIKANO, Toshio SHIGEMATSU1993 Volume 42 Issue 4 Pages 229-233
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWe studied an analytical method for determining ultra-trace Cu on silicon wafer by neutron activation analysis. First, we estimated the amount of contamination received from packing materials during irradiation in a nuclear reactor. Surface metal concentrations of 4 kinds of fluoride polymer film and 2 kinds of polyethylene film were determined by neutron activation analysis. We concluded that high-density polyethylene film is a suitable material for packing material and the amount of Cu contamination from this film is estimated to be below 1010 atoms cm-2. Then, we determined the amount copper on a silicon wafer. We found that the contamination during irradiation is below 6×109 atoms cm-2. The wafer, which has been spin coated with a Cu solution of 0.1 to 40 ppm, was also analyzed. A good linearity of solution concentration and surface concentration of Cu was obtained. The intentionally contaminated wafer of a desired concentration can be produced. The detection limits of Cu is 4×109 atoms cm-2 by instrumental analysis with a well Ge detector and is improved by utilizing chemical separation and a low background gas flow counter.View full abstractDownload PDF (738K) -
Kunihiro WATANABE, Satoshi MORIKANI1993 Volume 42 Issue 4 Pages 235-241
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFive Schiff bases, which were derived from 2-hydroxyaniline-N-salicylidene (HS), were synthesized in order to get excellent fluorescence-reagents having sulfo substituents. They are 2-hydroxy-5-sulfoaniline-N-salicyfidene (HSS), 2-hydroxyaniline-N-2-hydroxy-5-sulfobenzylidene (HSB), 2-hydroxy-5-sulfoaniline-N-2-hydroxy-5-sulfobenzylidene (HSSB), 2-hydroxy-5-sulfoaniline-N-2-hydroxy-5-chlorobenzylidene (HSCB) and 2-hydroxy-3-sulfo-5-chloroaniline-N-salicylidene (HSCS). The Al complex with HSB, which has a sulfo substituent in the methyne-side ring, did not show a remarkable enhancement of fluorescence, as compared with that of HS. The Al complex with HSSB, which has sulfo substituents in both methine-side ring and nitrogen-side ring, increased the fluorescence intensity as strong as the Al complex with HSS. HSCB and HSCS were superior to other four kinds of Schiff base on the fluorescence intensity of the Al complexes. The effect of the sulfo substituent in the Schiff bases on the fluorescence of their Al complexes was estimated under the condition of water-glycerin media as a function of viscosity by measurements of relative fluorescence intensity, fluorescence quantum yield, fluorescence life time and phosphorescence spectra at 77 K. The fluorescence intensity of the Al complex having one or two sulfo substituents was controlled by the energy level of electron in the Schiff base complex. As a result, the energy level was influenced with the position of the substituents rather than the kind of substituent.View full abstractDownload PDF (897K) -
Yasuo HAYASHI, Kiyoshi MATSUMOTO1993 Volume 42 Issue 4 Pages 243-247
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAnalysis of Na and H depth profile in SiO2 matrix using secondary ion mass spectrometry (SIMS) has been investigated. In general, migration of an analyte species, such as alkali elements in insulators, can occur during SIMS analysis because of the formation of an electric field and/or the thermal heating. This phenomenon distorts the depth profile, so that it is difficult to evaluate an accurate concentration distribution of elements, especially Na and H. In this study, use of the sample cooling during analysis has been found to eliminate successfully these migrations, since the mobility of elements decreases by the cooling. Furthermore, it was recognized that the detection limit of H was improved by the cooling because of an improvement of the vaccum in the analysis chamber. The developed technique can be applied to sodium silicate glasses to give more accurate depth profile.View full abstractDownload PDF (684K) -
Yukiko OKADA, Shoji HIRAI1993 Volume 42 Issue 4 Pages 249-254
Published: April 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSUltratrace amounts of uranium and thorium in high purity aluminium were determined by radiochemical neutron activation analysis (RNAA). The aluminium plate samples (ca. 110 g) were irradiated by thermal neutron flux of 4×1012 n cm-2 s-1 for 510 h at Musashi Institute of Technology Research Reactor (MITRR). After several days the irradiated samples were dissolved in 9 M HCl for anion exchange chromatography. 239Np and 233Pa adsorbed on the anion exchange resin from 9 M HCl were selectively eluted with 9 M HCl-5 M HF solution. By the addition of LaCl3 solution to this eluate, 239Np and 233Pa coprecipitated LaF3. γ-Rays from the coprecipitate on a filter paper were measured for determination of uranium and thorium. Several ppt levels of uranium and thorium were able to be determined by this method. Before RNAA the samples were nalyzed by INAA to evaluate analytical accuracy of the RNAA method. Influence of sample weight to geometric counting efficiency was corrected in the calculation of radioactivities of 239Np and 233Pa from γ-counting data. The analytical results obtained by RNAA indicated excellent agreement with the INAA results.View full abstractDownload PDF (920K) -
Mikito KAMIJO, Shizuo IKUNO, Takeshi YAMANE1993 Volume 42 Issue 4 Pages 255-258
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMonitoring system for detecting the reducing end point in gold recovering system is presented by using the reaction heat measurement as chemical probe. Sodium hydrogen sulfite was selected as reducing agent for gold(III) among the various agents examined, which yielded gold precipitation quantitatively. The reducing solution was pumped at a flow rate of 36 ml/min to the reaction vessel containing gold(III) solution and the increase in temperature was measured using thermistor detector. A linear relationship was observed between the gold(III) concentration up to 135 gAu/l and the increase in temperature. The relative standard deviation of recovered gold was 0.13% (n=4) for 60 g gold. The results of recovered gold mass from industrial waste in accessary factories agreed well with the one calculated from the increase of temperature.View full abstractDownload PDF (469K) -
Jun-ichi KAWAHARA, Shigeru HATTORI1993 Volume 42 Issue 4 Pages T49-T55
Published: April 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn order to contribute to the fundamental methodology on the accuracy and the reliability of light scattering measurements, a typical light scattering photometer (FICA type) was evaluated in detail, from the viewpoint of the angle scanning and the related properties. It was shown that, in immersion type light scattering photometers, optical alignment could be achieved with high accuracy by rather simple operation, so that the variation of cell constant is negligible between different observation angles, and that stray light is not so significant even at low and high angles. The principal cause of stray light is the difference of refractive index at the cell-solution interface, and it can be suppressed by appropriate selection of solvent or cell material. Although angular preciion around 0 deg is better than ± 0.007 deg, special care is necessary in the measurement of transmitted primary beam.View full abstractDownload PDF (1118K) -
Teiko OHMORI1993 Volume 42 Issue 4 Pages T57-T64
Published: April 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTwelve metallic elements in rain water were determined by ICP-AES. One hundred milliliters of rain water was collected for every one mm of rainfall with a fractional collector placed on the rooftop of a tall building which is about 30 m high in Funabasihi City, Chiba. The rain water was filtrated through membrane filter (0.45μm) and concentrated 10 times with a rotary evaporator before ICP-AES measurements. Both filtrate and the suspended solids were analyzed by ICP-AES for the metallic elements after decomposing with HCl-HF mixture. It rained 30 times from January to August in 1991 and it was collected. Changes in the metal contents of rain water during one rainfall and relationship between metal contents and pH value were discussed.View full abstractDownload PDF (991K)
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