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Volume 36, Issue 7
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Yasuko NODA1987 Volume 36 Issue 7 Pages 403-406
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSurface charge on the liposome formed from purified phospholipids was determined by colloidal microtitration with potassium polyvinylsulfate (PVSK) and polydiallydimethylammonium chloride (Cat-Floc). The end point was detected by the color change of 0.1% TB from blue to red-violet. A micro colloidal titration apparatus (Gilmont ultra-precision micrometer syringe, No. S3200) was used for titration. Phospholipids used in this experiment were as folows: phosphatidylcholine (PC), phosphatidylglycerol (PG), phosphatidylethanolamine (PE) and phosphatidylserine (PS). The chloroform solution of the phospholipid was transferred into a 25-ml stoppered teat tube and evaporated to dryness in vacuo at 3536°C. The thin film of the phospholipid in the vessel was suspended in distilled water (20 mg of lipid/2 ml) by sonicating for 30 min at room temperature. Stability of the liposome, whcih is a closed system composed of the lipid bilayer, was checked by using liposome entrapping glucose. From the results of colloidal titration, the surface of PC liposome was found not to be charged over the pH range from 2 to 11. This is considered due to formation of the intramolecular salt linkage between the phosphate group (pKa_??_2) and quarternary ammonium group of choline (pKa_??_13). PG liposome was negatively charged at above pH 3 with a constant value, (0.633±0.020) × 10-6 eq/10-6 eq of phosphorus. The plots of the equivalent of negative charge against the amount of phospholipid gave a straight line. The results of three separate determinations indicated good reproducibility. PE liposome showed a constant value, 0.646×10-6 eq/10-6 eq of phosphorus, at above pH 10.5. In the case of PS liposome, the constituent ratio of the functional groups was well corelated to the results of colloidal titration. From the constant values in the pH range of 6 to 7 and 10 to 11, the amounts of negative charge of the carboxyl and phosphate groups were determined as 0.541 and 0.546 ×10-6 eq/1 0-6 eq of phosphorus, respectively. This negative charge of the liposome was considered to reflect the surface charge of the closed vesicle of the bilayer of the phospholipids. Colloidal micro-titration is useful not only for detecting the state of the functional groups over a wide pH range, but also for quantitative determination of the negative charge on the surface of a small amount (0.5 to 1.0 mg of lipid/sample) of the phospholipid liposome.View full abstractDownload PDF (574K) -
Yasuyuki MIURA, Kohji TATEGAMI, Tomozo KOH1987 Volume 36 Issue 7 Pages 407-411
Published: July 05, 1987
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA method has been developed for the determination of micro amounts of hexathionate. It is based on the reaction of hexathionate with a given amount of permanganate in a dilute sulfuric acid medium and on the spectrophotometric measurement of iodine (as triiodide), which is formed by the oxidation of iodide with an excess of permanganate. When the mixture of 1.5 ml of 1 M sulfuric acid, 4 ml of 2 × 10-4 M permanganate and 10 ml of hexathionate solution was allowed to stand for 20 min at temperatures ranging from 5 to 40°C, 2 mol of hexathionate was oxidized stoichiometrically with 9 mol of permanganate. The present method could be successfully applied to a determination of hexathionate in the range from 1.8 × 10-7 to 1.1 × 10-5 M (0.531.7 μg S6O62- in 10 ml) and gives a higher sensitivity than any previous method without solvent extraction. From eleven measurements for 10 ml of sample solution containing 5.00 × 10-2μmol of hexathionate, the mean value was 5.02 × 10-2 μmol with a standard deviation of 3.2 × 10-4 μmol and a relative standard deviation of 0.63%.View full abstractDownload PDF (866K) -
Takako NISHIKAWA, Keiichiro HOZUMI1987 Volume 36 Issue 7 Pages 412-415
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSOrganic samples containing mineral constituents have been ashed in a chamber of a glow discharge of oxygen at relatively low temperature, but significantly low recovery was obtained when chloride-containing samples were ashed and analyzed. A considerable amount of chlorate was also found in the ash material. Such unusual behavior was attributed to highly energetic electron impact and ion bombardment onto the surface during the period of ashing within the glow discharge region. To eliminate the charged particles from the oxygen plasma and oxidize the sample with practically pure atomic oxygen, a novel design of plasma chamber was proposed. A stainless steel basket was tightly inserted into the plasma chamber facing the bottom of the basket closely to the plasma exciter. A sample boat was placed inside the metal basket and the ashing was carried out. No glow discharge was observed inside the basket because of the electrostatic shielding from the radio frequency coil. Electrons and ions produced in the glow discharge region were effectively neutralized at the surface of the metal mesh, while the atomic oxygen freely flowed in the basket to oxidize the sample. Nearly quantitative recovery of chloride was obtained by ashing a few organic materials in the modified plasma chamber while negligible amount of chlorate was found as the component.View full abstractDownload PDF (537K) -
Qi WENQI, Fu-Sheng WEI, Keiichi FURUYA, Yohichi GOHSHI1987 Volume 36 Issue 7 Pages 416-419
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA procedure was studied for direct determination of trace Li in serum by graphite furnace AAS. Ammonium sulfate was used as a matrix modifier and the optimum ashing and atomizing temperature were established to suppress effectively the matrix effects caused by coexisting protein and chloride ion. The background absorption was corrected using a Zr line at 670.2 nm, appropriately adjacent to the analytical line of Li at 670.8 nm. The dynamic range of this method is given by two linear calibration curves corresponding to 0.0430 ppb and 303000 ppb. The method was successfully applied to the serum samples of healthy persons and mental patients and gave satisfactory results.View full abstractDownload PDF (592K) -
Koichi AOKI, Kazunobu MAEDA, Koichi TOKUDA, Hiroaki MATSUDA, Kiyoshi H ...1987 Volume 36 Issue 7 Pages 420-424
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe current response to the potential square-wave with large amplitude and large effective potential scan rate exhibits a bell-shaped voltammogram, which is independent of electrode geometry and of which area compassed by a base line is proportional to the square-wave amplitude. The proportionality of the area to the amplitude was explored in a solution of K3Fe (CN)6 (10-75 × 10-4 mol dm-3) at the carbon fiber electrodes, which have often been used as an in-vivo electrochemical detector. Since the voltammogram at 10-7 mol dm-3 analyte was largely deformed from the ideal bell shaped one due to involvement of electric noises and residual currents, it was difficult to discern a peak current and peak potential visually from the voltammogram. The proportional constant, however, could be evaluated readily by plotting the peak area against the amplitude. The proportional constant was in good agreement with the value calculated from the diffusion coefficient and electrode area. Square-wave experiment with variation of the amplitude is a promising analytical technique of enhancing S/N ratios.View full abstractDownload PDF (679K) -
Masayo MUROZUMI, Seiji NAKAMURA, Shinichiro KAWAHARA1987 Volume 36 Issue 7 Pages 425-430
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIsotope dilution surface ionization mass spectrometry has been applied to the accurate determination of Tl, Ag, Cu, Cd, Pb, Ni and Zn in standard reference materials. After being spiked with 203Tl, 107Ag, 65Cu, 116Cd, 206Pb, 61Ni and 68Zn, the spiked sample was decomposed with a mixture of HNO3, HClO4 and HF at low temperature under pressure and the digest was evaporated to dryness under nitrogen. The residue was dissolved in dilute HNO3 solution. The heavy metals were extracted from the solution as their dithizonates into chloroform. An aliquot was applied to the mass spectrometer (Hitachi RMU-6) equipped with a surface ionization device incorporating a Re single filament. With raising the temperature of ionization filament, the mass spectrometer could measure successively the wide range of isotopic ratio of the spiked elements within 1% relative standard deviation. The present method could determine minute amounts, i.e., 10-910-11 g of the above elements with a precision of 1%.View full abstractDownload PDF (884K) -
Relation between the decreasing rate of particle number density and particle sizeHiroshi KAWAGUCHI, Katsuyoshi KAMAKURA, Eiji MAEDA, Atsushi MIZUIKE1987 Volume 36 Issue 7 Pages 431-435
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSParticle number densities, n and size distributions of an aerosol filled in a cylindrical metal vessel (volume: 7 l) were periodically measured by the direct aerosol introduction/ICP-AES described previously. The aerosol were prepared with powders of various calcium compounds or glasses to measure the emission intensities at Ca II 393.37nm. The decreasing rate of log(n) was constant for each fraction of particle size of a given compound and the values agreed reasonably with the theoretically calculated values. By this method, the pulse height spectra obtained by the ICP-AES of aerosols of unknown composition particles containing calcium can be related to the size distribution curves.View full abstractDownload PDF (643K) -
Qi WENQI, Keiichi FURUYA, Yohichi GOHSHI1987 Volume 36 Issue 7 Pages 436-440
Published: July 05, 1987
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA precise analytical method for using graphite furnace AAS is described for the determination of trace amounts of Co and Ni in plant materials. By adding NH4VO3 as a matrix modifier, direct quantitative determinations of Co and Ni are possible without preconcentration or separation of coexisting elements. This method was applied to the determinations of Co and Ni in Tea and Orchard Leaves (NBS SRM 1570) with satisfactory results. The analytical results of Co were 0.19μg/g and 1.35μg/g on the average for Orchard Leaves and Spinach, respectively, which agreed with the reference value (0.2μg/g and 1.5μg/g). The results of Ni were 1.22μg/g and 5.68μg/g respectively on the average for Orchard Leaves and Spinach, which agreed with the value 1.3±0.2μg/g and reference value 6μg/g.View full abstractDownload PDF (760K) -
Satori UTSUMI, Junichi YAMAGUCHI, Akinori ISOZAKI1987 Volume 36 Issue 7 Pages 441-446
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSBromide ion is oxidized to bromine with potassium permanganate in sulfuric acid solution, and iodide ion to iodine with hydrogen peroxide. The liberated bromine or iodine is extracted with carbon tetrachloride and back-extracted into an acidic aqueous phase containing Bindschedler's Green Leuco base (BGL), forming quantitatively BG+ which has an absorption maximum at near 720 nm. The analytical procedure for bromide ion is as follows. To 10 ml of a sample solution containing less than 3 ppm Br- in a separatory funnel, 1 ml of 3.0 M sulfuric acid and 1 ml of 0.015 M potassium permanganate are added. After standing for 5 min, 5 ml of carbon tetrachloride is added to the funnel and it is shaken for 30 s. The organic phase is transferred to another funnel and 5 ml of 0.5 M sulfuric acid is added. The mixture is shaken for 30 s to wash the organic phase. Then, the organic phase is transferred again to another funnel and 10 ml of 2.0 × 10-4 M BGL (pH 1.2) is added. The mixture is shaken for 30 s to make bromine react with BGL. The absorbance of BG+ in the aqueous phase is measured at 715 nm with a 1 cm cell against water. For the analytical procedure of iodide ion, 1 ml of 4.5 M sulfuric acid and 1 ml of 3% hydrogen peroxide are added to 10 ml of a sample solution containing less than 4 ppm I- in a funnel, and it is allowed to stand for 5 min. The subsequent procedures are the same as those for bromide ion described above, except for washing of the organic phase with 5 ml of 0.05 M sulfuric acid and for the back-extraction with 10 ml of 2.0 × 10-4 M BGL (pH 4.0) and for the measurement of absorbance at 725 nm. The effect of foreign ions was examined, and the methods for bromide and iodide ions were applied to natural water samples. The relative standard deviation for the determination of 62.3 ppm bromide ion in standard seawater sample was 1.4% (n=10).View full abstractDownload PDF (797K) -
Hiroaki TAO, Takashi IMAGAWA, Akira MIYAZAKI, Kenji BANSHO1987 Volume 36 Issue 7 Pages 447-450
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAtmospheric pressure helium microwave induced plasma sustained with a Beenakker type cavity (He-MIP), which is very useful for the determination of metallic and non-metallic elements, has not yet been applied to volatile β-diketonates. The purpose of this work is to investigate optimum conditions for the determination of Be and Cr acetylacetonates with GC/ He-MIP emission spectrometry. A OV-1 coated fused silica capillary column (0.53 mm i. d., 10 m long, 2μm film thickness) and a TM010, Beenakker type cavity were used. The most critical parameters were plasma power and plasma gas flow rate. Optimum conditions for Be II 313.01nm (these two lines could not be resolved with a monochromator used) with 1 mm i.d. discharge tube were as follows: microwave power, 60 W (10 W reflected); carrier gas flow rate, 15 ml/min; plasma gas flow rate, 600 ml/min. In general, gas flow rate influenced emission intensities of ionic lines more severely than those of atomic lines. Each special distribution of emission intensity of Be II 313.0 nm, Be I 234.9 nm and He I 388.9 nm was different. The linear dynamic range was almost 104, and the limits of detection (S/N=3) were 0.1 pg for Be and 9 pg for Cr, respectively. The relative standard deviation was 11 % at 1.7 pg of Be.View full abstractDownload PDF (576K) -
Kenjiro HAYASHI, Yoshiaki SASAKI, Shoji TAGASHIRA, Yoshiko MURAKAMI, K ...1987 Volume 36 Issue 7 Pages 450-452
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAmmonium 1-pyrrolidine dithiocarbamate (NH4pdtc) was used for a gravimetric determination of Cu(II). Cu(II) ion in the solution was quantitatively precipitated as [Cu(pdtc)2] in the pH range 112, when a small excess of NH4pdtc solution was added. The precipitate was not decomposed at 60°C for 6h in contact with mother liquor, and was stable on heating up to 140°C after filtration. The procedure for the determination of crystalline copper(II) sulfate was following: crystalline copper(II) sulfate (containing 10100mg of copper) was dissolved in 200cm3 water, a 0.1% NH4pdtc solution was added to the solution until precipitation was completed. After the adjustment of pH to 8.09.5, the mixture was allowed to stand at 60°C for 1h. The precipitate was filtrated, washed with hot water, dried at 110°C, and weighed. This method is accurate and precise, e.g., the mean of relative errors and the relative standard deviation obtained for 20mg of copper were 0.1% and 0.1% (n=6), respectively. This method is suitable for standardizing a Cu(II) solution containing no other heavy metal ion.View full abstractDownload PDF (530K) -
Hiroshi KAWAGUCHI, Yoshinori HOTTA, Atsushi MIZUIKE1987 Volume 36 Issue 7 Pages 453-455
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn image dissector tube with a slit aperture (17μm ×3mm) was attached to a 1-m Ebert type spectrograph whose plate holder and racking mechanism were removed. Almost flat responses were obtained along the horizontal axis of the photocathode (16mm long, spectral range 7.4nm). Spectral signals were measured by dc amplification, phase sensitive amplification with wavelength modulation, or digital integration with a transient memory and a signal averager. The first method was most unfavorable as for the detection limits, the second was convenient for the automatic background correction, and the third was useful for qualitative and multielement analysis. Detection limits were nearly the same for the last two methods but worse by one order of magnitude than those by the conventional method with a photomultiplier.View full abstractDownload PDF (367K) -
Kei YAMADA, Osamu KUJIRAI, Muneyuki KOHRI, Kunikazu IDE, Haruno OKOCHI1987 Volume 36 Issue 7 Pages T67-T71
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSReaction solutions (sample solutions) of lead-removed residue of lead concentrate which were oxidized by potassium permanganate in hydrochloric acid solution were analyzed by ICP-AES using internal standard method. The sample solutions contain widely varying concentrations of S, Fe, Mn, Zn, Cu, Pb, Al, Mg, Si, K and Na. The sample solutions were prepared in 2- and 10-fold dilute solutions. Calibration and synthetic sample solutions (2- and 10-fold dilutions) were matrix-matched for the sample solutions. Satisfactory accuracy and precision were obtained for the 9 elements except for sodium and potassium using 10- and 2-fold dilute solutions of the synthetic sample solutions.View full abstractDownload PDF (807K) -
Application of background correction and band fitting to Raman spectraKatsuo MURATA, Donald E.IRISH1987 Volume 36 Issue 7 Pages T72-T76
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to understand hydrothermal chemistry in the earth, iron(III)-chloro complex solutions were examined at elevated temperatures and pressure by using Raman spectroscopy. A portion of five molal hydrochloric acid solution of 1.0m (= mol kg-1) FeCl3·6H2O was injected into the Corning capillary glass. Raman spectra of sample solutions at elevated temperatures were obtained using the furnace under the pressure of 9 MPa. The background correction using the PETEXPOL program was applied to the Raman spectra obtained. Then the band fitting of overlapping lines was performed with the PETBNDFT program operating on an IBM 4341 computer. These analyses showed that iron (III)-Cl solution is a mixture of the octahedral and the tetrahedral iron(III) chloro complexes at 100 °C, but that the tetrahedral FeCl4- species is preferential at 300 °C.View full abstractDownload PDF (602K) -
Kazuo WATANABE, Misao OUCHI1987 Volume 36 Issue 7 Pages T77-T80
Published: July 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSimple procedure for the preparation of sulfur dioxide from sulfate was developed and applied to the determination of sulfur in steels by isotope dilution mass spectrometry. Sulfur in sulfate was recovered as 2-perimidinylammonium sulfate. The recovered precipitate was thermally decomposed by heating under vacuum at 450 °C for 5 min to yield sulfur dioxide which was used for subsequent mass spectrometric isotope analysis. Steel samples were dissolved in a sealed polytetrafluoroethylene vessel to convert all sulfur into sulfate using nitric and hydrochloric acids. Iron was removed by extraction with 4-methyl-2-pentanone prior to precipitation of the sulfate. The results on JSS standard samples were in good agreement with the standard values. The relative standard deviation was less than 5% for sulfur contents in the range of 0.00140.019%.View full abstractDownload PDF (702K)
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