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Volume 37, Issue 3
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Katsushige TAKAMI, Tameo OKUMURA, Hiroyasu YAMASAKI, Masao NAKAMOTO1988 Volume 37 Issue 3 Pages 117-122
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSOrganotin compounds (OTC) in polyvinyl chloride (PVC) products were converted to their propyl derivatives and determined simultaneously with a GC apparatus equipped with a flame photometric detecor (FPD). A 0.1 1.0 g amount of a PVC sample was dissolved in 15 ml of tetrahydrofuran(THF) under refluxing condition for 1 h. The THF extract was made up 20 ml with THF. A 0.1 5 ml volume of the extract (containing below 5 μg of OTC) was mixed with a 25 ml volume of 2 M propylmagnesium bromide (PMB) THF solution and allowed to stand for 30 min. The excess PMB in the mixture was deactivated by adding 10 ml of 0.5 M sulfuric acid. The mixture was filtered, and the residue was washed twice with 5 ml of ethanol. The propyl derivatives (Rn-Pr4-nSn) in the combined filtrates, mixed with water, was extracted with hexane. The hexane extract was dehydrated with anhydrous sodium sulfate, filtered and concentrated to 5 ml. An aliquot of the concentrated sample was analyzed by GC with FPD which was equipped with a 600-nm cut-on interference filter to monitor the tetraalkyltin compounds. GC conditions were as follows: column, Ultra-2 (crosslinked 5% phenyl methyl silicone gum, 0.32 mm i.d. × 25 m, df=0.52 μm), column temp. = 70°C (4 min)-4°C/min-240°C, helium (2 ml/min), injection and detection temp. = 260°C, split ratio= 1/4. OTC in the PVC products were identified on the basis of retention times and determined by peak height method. Recoveries of OTC from a PVC resin product were 88.399.6% and relative standard deviations were 2.76.8%. The detection limits of OTC were 0.1 ng as their chloride. The limit of determination was 2μg/g, when 1 g of the resin was analyzed.View full abstractDownload PDF (951K) -
Shinobu SHIMIDZU, Hidetoshi ARAKAWA, Masako MAEDA, Akio TSUJI1988 Volume 37 Issue 3 Pages 123-127
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA highly sensitive chemiluminescent assay for invertase activity by using lucigenin has been developed, and was applied to chemiluminescent enzyme immunoassay with invertase as label enzyme. Invertase is an enzyme that catalyses the hydrolysis of saccharose of form glucose and fructose. By adding lucigenin solution into the hydrolyzed solution, intensive light was produced. The procedure for the assay of invertase activity is as follows: the mixture of 0.1 ml of invertase 0.2 ml of 0.3M saccharose solution and 0.2 ml of 0.25 M acetate buffer (pH 5.0) was allowed to stand at 4°C, over night, and after 0.1 ml of 0.5 M phosphate buffer (pH 7.0) was added. The mixture was heated for 1 min in boiling water. Aliquot of 0.1 ml of this reaction mixture was assayed by adding lucigenin solution (1.2 × 10-3% lucigenin -1 × 10-3 M Triton X-100 -0.16 M KOH). The light intensity was measured with a luminometer (waiting time, 15s, integrating time, 1530 s). A log/log linear relationship between the chemiluminescence intensity and invertase activity was obtained from 102 to 104 μU/ assay, and the detection limit of invertase by this reaction was about 10-15 mol. The relative standard deviation of invertase was 1.75.9% (n=10). And a new chemiluminescent enzyme immunoassay of 17α-hydroxyprogesterone and thyroxine were developed by using invertase as label enzyme. The measurable ranges of 17α-hydroxyprogesterone and thyroxine were 10 to 500 pg and 25 to 500 pg/assay, respectively. The 17α-hydroxyprogesterone values in serum samples were assayed by both fluorescent and the present methods. The results showed good correlation ( Y (proposed enzyme immunoassay) = 0. 81X (fluorescent enzyme immunoassay) + 0. 11, r = O. 90, n = 30).View full abstractDownload PDF (638K) -
Tomoo MIWA, Xin-gen YU, Atsushi MIZUIKE1988 Volume 37 Issue 3 Pages 128-132
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAbout 36mg of Ta is anodically dissolved from the surface of a helical wire sample (0.5 mm diam. × 200 mm) in 200μl of 5 M hydrofluoric acid-1M nitric acid-1.75 × 10-4 M Hg (II) electrolyte by constant current electrolysis at a current density of about 8 mA/cm2 for 510 min using a glassy carbon cathode. After replacement of the sample by a Pt anode, greater than 95% of Cu in the electrolyte is electro-deposited together with Hg on the glassy carbon cathode at -0.7Vvs. SCE within 10 min for differential pulse anodic stripping voltammetry. Fractional μg/g of Cu in high-purity Ta wire is determined, with a relative standard deviation of about 5%, by the proposed method within an hour. In the stripping voltammetric determination of trace impurities in high-purity solid materials, use of microliter electrolytes is more favorable than conventional techniques using milliliter electrolytes from the viewpoints of sensitivity, precision and rapidity, provided that appropriate apparatus are devised to overcome operational difficulties due to miniaturization. Another advantage of microscale techniques is minimization of high-purity reagents consumption and experimental wastes.View full abstractDownload PDF (596K) -
Toyoaki AOKI, Koichi ITO, Makoto MUNEMORI1988 Volume 37 Issue 3 Pages 133-136
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSample solution, pumped at a flow rate of 5.2 ml min-1, is continuously mixed with 0.25 M sulfuric acid, and is then led to a debubbler to remove inorganic carbonate from the sample solution. The sample solution is then mixed with 7% alkaline peroxodisulfate solution which flows at a flow rate of 2.6 ml min-1, followed by heating in a reaction coil (8000 mm × 1.5 mm i. d.) kept at 210°C. In this process, inorganic carbonate is produced by oxidation of the organic species by alkaline peroxodisulfate. The inorganic carbonate thus formed is mixed with 3 M sulfuric acid to convert to carbon dioxide and is fed to a double-tube separation unit (an inner tube: 1.8 mm o.d., 1.0 mm i.d., length 500 mm microporous PTFE; an outer: 4.0 mm o.d., 2.5 mm i.d., length 500 mm Pyrex), where the carbon dioxide in the outer tube permeates through the microporous PTFE membrane and reacts with luminol reagent (1 mM luminol, 20 mM H2O2, 0.02 mM CoCl2, and 10 mM borate at pH 9.0) which flows in the inner tube at a flow rate of a 0.22 ml min-1. The chemiluminescent intensity is measured with a photomultiplier tube.Phthalate, amino acids, ethanol, dextrose, and starch were almost completely converted to carbon dioxide by the present method. The response was obtained within 11 min. The calibration curve was linear over the concentration range from 0.06 to 12 C-ppm, and the detection limit (S/N = 3) was 0.03 C-ppm. The relative standard deviation (n=5) was 1.5% for 4.8 C-ppm. Inorganic salts commonly present in river and seawaters did not interfere with the determination.View full abstractDownload PDF (585K) -
Automatic photometric titration of surfactants based on two-phase titration; IVSatoshi TAKANO, Akira HASEGAWA, Hiroshi OHOTSUKA1988 Volume 37 Issue 3 Pages 137-141
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of soap in anionic surfactant mixtures and amine and quaternary ammonium salts in cationic surfactant mixtures was carried out by using an automated photometric titrator equipped with porous PTFE (Teflon) membrane separator (previous publications) based on two-phase titration. In the case of soap in anionic surfactant mixtures, it is necessary to determine surfactant mixtures under both acidic and alkaline conditions, and the difference between the two determinations indicates the content of soap. However, the analytical values of some anionic surfactants (sodium alkanesulfonate and α-olefinesulfonate) under acidic and alkaline conditions by the previously proposed method were found not to be identical. The difference was considered to be caused by the presence of polysulfonate. Therefore, 7% of 1-hexanol was added to chloroform to improve the recovery of polysulfonate. Under these conditions, the determination of soap in anionic surfactant mixtures was successfully carried out. Furthermore, sulfate-type anionic surfactants in anionic surfactant mixtures were determined by the acid hydrolysis method. By the same way as anionic surfactants, the determination of cationic surfactant mixtures (amine and quaternary ammonium salts) could be also effected by using Disulphine Blue as an indicator, which could be used under both acidic and alkaline conditions.View full abstractDownload PDF (762K) -
Junichi KOYAMA, Takashi MATSUMOTO, Yutaka OHTSU, Okitsugu NAKATA1988 Volume 37 Issue 3 Pages 142-146
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and simple method by using HPLC was developed for the determination of thioglycolic acid, dithiodiglycolic acid, cysteine and cystine in hair-waving solutions. Ion pair method was suitable for the separation of these ingredients. HPLC conditions used for the separation were: column packing and size, CAPCELL PAK C18 and 4.6 mm i.d. × 250 mm;mobile phase, a mixture of 5% acetonitrile-95% water contained 0.1% phosphoric acid and 3.5 mM 1-heptanesulfonic acid; detection, UV 210 nm. Recoveries of these four ingredients from the model sample were 100102%. p-Hydroxybenzoic acid (0.25 mg/5 ml) was added to 0.25 g of sample as an internal standard and then it was diluted to ca. 40 ml with water; 10μl of this sample solution was injected into chromatograph. By using this method, the four ingredients in 9 commercial hair-waving solutions were accurately determined without interferences of other ingredients.View full abstractDownload PDF (765K) -
Keiko OHSAWA, Katsumi UCHIYAMA, Shinichi SUZUMURA, Kazuo IMAEDA, Kohei ...1988 Volume 37 Issue 3 Pages 147-151
Published: March 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSProteins and DNA-fragments electrophoresed on the slab gel were determined by use of light scanning photoacoustic densitometer. Proteins were separated. by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The silver staining procedure was improved from Oakley's method. DNA-fragments were separated by agarose gel electrophoresis. Willoughby's method was used as the silver staining for DNA. Photoacoustic densitometer which was newly constructed, was composed of a He-Ne laser as a light source, light chopper, X-Y table, photoacoustic cell, lock-in amplifier, microcomputer and recorder. The scan of the light beam was controlled with a microcomputer. Sensitivity of the modified silver staining for proteins was about 50 times greater than that of Amide Black 10B and 1.5 times greater than that of Oakley's method. Reproducibility of measurement by the modified method was comparable to the dyeing method. Sensitivity of Willoughby's method for DNA-fragments was about 20 times greater than that of the Toluidine Blue-O method. Reproducibility of measurement by Willoughby's method was not satisfactory.View full abstractDownload PDF (710K) -
Yutaka OKAUE, Yasuhiro YOSHIOKA, Masato HIRANO1988 Volume 37 Issue 3 Pages T41-T44
Published: March 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA novel method for depth profiling of polymer content of polymer-polymer mixtures has been developed by using ultramicrotome surface slicing technique combined with electrophoresis and densitometry analysis. A gelatin bilayer film was used containing a betaine type polymer in the upper layer as a model system. By microtoming the film surface as thin as 1μm from the top to the bottom successively, a series of microtomed slices could be obtained. Depth profiling was achieved by analyzing each microtomed slice using electrophoresis and densitometry. This method might be applied to depth profiling of various types of multilayer films containing different additives by utilizing IR, SIMS, or Raman analysis instead of the above detection methods.View full abstractDownload PDF (613K) -
Kunio TAKADA, Hideyuki KONNO, Tsutomu SYOJI1988 Volume 37 Issue 3 Pages T45-T49
Published: March 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe determination procedures of a major component of a rare earth element (RE)-Rh-B compound were investigated. The REs used were Ce, Nd, Sm, Gd and Er. The sample (0.08 to 0.15 g) was dissolved in aqua regia. The RE and Rh were removed as the hydroxides from B in the range of pH 9.8 to 10 with NaOH. Boron was titrated in the presence of mannitol with 0.05 M NaOH solution. Rare earth element and Rh hydroxides were dissolved in HClO4. Rhodium (III) was reduced to metallic Rh by adding excess metallic Zn, about 2.5 g. The residual Zn was dissolved with HNO3. Rhodium was filtered off, burnt to ash, heated for 3 h at 1080 °C in air and then weighed as metallic Rh. The RE in the filtrate was precipitated as the fluoride, filtered off, converted to the oxide by fuming with HClO4 and drying, dissolved in HCl and then titrated with 0.02 M EDTA solution. Copper and Al existing as impurities in the sample were determined by flame AAS. The sum of percentages for five elements (RE, Rh, B, Cu and Al) found in the sample was substantially 100%.View full abstractDownload PDF (751K) -
Yoshiro MATSUMOTO, Mamoru YAMAJI, Nobukatsu FUJINO1988 Volume 37 Issue 3 Pages T50-T54
Published: March 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn XRF analysis of iron ores, FeKα intensity is influeneced by coexisting impurities and the loss of bound water as well as the gain of oxygen in glass bead preparation. In general, the internal effect can be corrected by the dj correction method. On the other hand, sodium tetraborate (Na2B4O7) is frequently used as a fusion flux. The ratio of Na2B4O7 to iron ore sample is usually adjusted to be 7-10:1 in Japan. The correction factors of JIS M 1256 method have been proposed by the authors for the proportion: 10 parts sodium tetraborate and 1 part sample. In this paper the correction factors dj were calculated for the proportion at 7 parts sodium tetraborate and 1 part sample. The values of the intensity correction factors, dj were 1.4 times larger than those of Na2B4O7:sample= 10:1. On the other hand, the correction factor could also be calculated by using the effective wavelength.View full abstractDownload PDF (664K)
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