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Volume 39, Issue 7
Displaying 1-13 of 13 articles from this issue
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Kunihiro WATANABE, Akane TSUTSUMI, Nobuyuki KOURA1990 Volume 39 Issue 7 Pages 375-380
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIn order to develop new reagents for catalytic analysis of cobalt, monoazo derivatives of 1-amino-8-naphthol-3, 6-disulfonic acid having electron-attractive or -donative groups were synthesized. Relationship between the structure of dyes and sensitivity for the catalytic analysis of cobalt was investigated. By following the Hammett's law, the fading rate of almost all of the examined dyes was accelerated by substitution of electron-donative groups in the dyes. The dyes having electron-donative groups were useful as the sensitive reagents for the catalytic analysis of cobalt. Further, the optimum conditions were investigated for the determination of cobalt with the most sensitive reagent, 1-amino-8-hydroxy-7-(p-hydroxyphenylazo)-3, 6-naphthalenedisulfonic acid (p-OH) among the examined dyes. The procedure was as follows: Take a sample solution containing less than 60 ng of Co (II), add 1.5 ml of 0.1 M Tiron solution and 5 ml of 3.5×10-4 M dye solution, and dilute the solution with water to a 50 ml after adjusting pH to 10.5. Then, circulate the solution through a flow cell in order to determine the absorbance with tube pump (flow rate: 2.5 ml/min). Add 2 ml of hydrogen peroxide solution (6.2%). Read the values (A1, A6) of absorbance after 1 min and 6 min, respectively. A calibration curve was constructed by relationship between ln (A1/A6) and the concentration of cobalt. The values of ln (A1/A6) were nearly proportional up to 1.2 ppb of cobalt, and the relative standard deviation was 6.9% (n=7) at 1 ppb of cobalt.View full abstractDownload PDF (983K) -
Kunio TAKADA, Mikio ISHIKURO, Minoru HOSOYA1990 Volume 39 Issue 7 Pages 381-385
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSTungsten in an intermetallic compound, Co3Ti, was determined by ICP-AES using carbon in tartaric acid as an internal standard. A sample of 0.1 g was dissolved with a mixture of nitric acid and hydrofluoric acid. Sulfuric acid was added and the content was heated to fumes. Tartaric acid was added to prevent from hydrolysis of W in the solution. The analytical lines of W II 207.911 nm and W II 209.475 nm were used. The atomic line of carbon (C I 193.091 nm) due to added tartaric acid was used as an internal standard. The effects of sulfuric acid and matrix elements on the intensity ratio of W to C were examined. The interfering effects by sulfuric acid (015 ml/100 ml) and Co (01 g) were corrected by the internal standard method. Interference of Ti on the determination of W was negligible because the Ti content was less than 25 mg in 0.1 g sample of Co3Ti. The relative standard deviation of this method was approximately 1% for the determination of 2.5% W in Co3Ti and the detection limit was 0.004% W for a 0.1 g sample of the material.View full abstractDownload PDF (814K) -
Kazuyoshi FUJIMURA, Tsuguo SAWADA1990 Volume 39 Issue 7 Pages 387-391
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe nitrogen oxides in flue gases were absorbed by the ozone oxidation method. A column used for the ion chromatographic separation was TSKgel IC-Anion-PW (4.5×50 mm). Phosphoric acid, borax, sodium loctanesulfonate, etc. were examined as an eluent. A mixture of 1 mM borax-75 mM boric acid-3.2 μM triethylenetetramine-N, N, N', N'', N''', N'''-hexaacetic acid hexasodium salt-0.2 mM triethylenetetramin-10% acetonitrile solutions showed the best separation. The detection limit (S/N=3) of nitrate ion was 2 ng/ml for a UV detector and 20 ng/ml for an electric conductivity detector, respectively.View full abstractDownload PDF (602K) -
Koichi YAMAMOTO, Koji IKEHARA, Shoji MOTOMIZU1990 Volume 39 Issue 7 Pages 393-397
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for spectrophotometric determination of anionic surfactants with Bromocresol Purple (BCP) and cetyldimethylbenzylammonium ion (CDMBA+) was developed. The addition of CDMBA+ to BCP solution buffered at pH 8 leads to a decrease in the absorbance at 588 nm. When anionic surfactants are added to the solution, the absorbance at 588 nm increases with increasing amounts of anioic surfactants. This increase in absorbance is caused by an ion association of CDMBA+ with anionic surfactants. On the basis of this principle, the simple spectrophotometric method for the determination of anionic surfactants was developed. The recommended procedure is as follows: Pipet an adequate amount of a sample solution containing anionic surfactants up to 1.7×10-5 M into a 10-ml volumetric flask. Add 0.5 ml of 4×10-4 M CDMBA solution, 1 ml of 1.7×10-4 M BCP solution and 0.5 ml of 0.2 M phosphate buffer solution(pH 8.1). Mix thoroughly and dilute to the mark with distilled water. Measure the absorbance of the solution at 588 nm against the reagent blank. The calibration graph shows linearity up to 1.7×10-5 M of anionic surfactants and the apparent molar absorptivity is about 6×104 l mol-1 cm-1. This proposed method is very simple and there is minimal interference from coexisting anions. The method also can be applied to the determination of anionic surfactants by a visual method.View full abstractDownload PDF (692K) -
Noriko OHNO, Tadao SAKAI, Masayuki NAKABAYASHI, Hideto SASAKI1990 Volume 39 Issue 7 Pages 399-403
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESS2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino) aniline (5-Br-PSAA) reacts with nickel to form a 2:1 complex (5-Br-PSAA: Ni). The absorption maximum of the complex is at 568 nm and the molar absorptivity is 1.17×105lmol-1cm-1 Nickel in the range of 0.04 to 0.5 ppm could be determined. The relative standard deviation was 0.72% for 10 determinations of 0.3 ppm nickel. The detection limit was 40 ppb. Most metal ions such as Al, Cr, Zn, Ca and Cd did not interfere at levels from 3 to 300 ppm. In the determination of 0.3 ppm nickel, the tolerance limits of copper, cobalt and iron were 30 ppb. However, interference from trace amounts of copper and iron could be depressed by addition of thiouria and Tiron. The method is applicable to the determination of trace amounts of nickel in an aluminium-based alloy not containing cobalt. Selective determination of trace amounts of nickel is also possible by adding thiouria and Tiron as masking reagents after removal of iron from some stainless steels in the HCl-MIBK extraction system. Moreover, the color development due to Ni-5-Br-PSAA complex formation can be introduced into FIA for reproducible determination of nickel.View full abstractDownload PDF (751K) -
Hiroaki MATSUURA, Katuji FUJIYAMA, Norio MINAGAWA, Junichi SAWA1990 Volume 39 Issue 7 Pages 405-409
Published: July 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA sensitive HPLC method with ultraviolet postcolurn-labeling using 2, 4-dinitrophenylhydrazone (DNPH) was developed for the determination of acetoin (AC), diacetyl (DA) and acetaldehyde (AA) produced by microorganisms in yoghurt and wine. A methanolic sample solution was prepared by mixing 10 g of these fermented foods with 50 ml of methanol. A reaction mixture was prepared by mixing 70 ml of methanol, 10 ml of hydrochloric acid, 50 mg of DNPH and 20 ml of anilin. One milliliter of the sample solution was added to 1 ml of the reaction reagent and the mixture was allowed to stand for 60 min at 27°C to form AC-DNPH, DA-DNPH and AA-DNPH derivatives. Twenty microliters of the reactant was injected into a reversed phase column with an aqueous solution of acetonitrile (water: acetonitrile=50:50). AC-DNPH, AA-DNPH and DA-DNPH were separated completely at 9, 13 and 15 min, respectively by HPLC monitored at 365 nm. Detection limits were about 0.050.1 μg for each of AC, DA and AA in 1 g of sample. The reproducibility of the HPLC measurements was 1.73.9% (R.S.D.). This method was applied successfully to the determination of AC, DA and AA in a variety of fermented foods.View full abstractDownload PDF (694K) -
Naoki HAMADA, Takao YAGI1990 Volume 39 Issue 7 Pages 411-414
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSystem peaks can be observed in nonsuppressor type anion chromatography using low pH eluent (pH<7). Since the analysis time depends on the elution time of the system peaks, methods to control the elution time of system peaks were studied. Usually, various bases are added to the mobile phase for pH control. It was observed that approximately linear relationship exists between the elution time of the system peak and acid dissociation constant (pKa) of the base. And the elution time of system peak could be freely controlled by changing component ratio of two different bases.View full abstractDownload PDF (481K) -
Kazuyoshi FUJIMURA, Tsuguo SAWADA1990 Volume 39 Issue 7 Pages 415-417
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSConcentration of nitrogen oxides in engine exhaust gases were determined by the use of ion chromatography. Nitrogen oxides, which were perfectly oxidized by the ozone oxidation method, in the range of ppm (v/v) level could be successfully determined with a UV detector.View full abstractDownload PDF (266K) -
Izuo AOKI, Kunihiro WATANABE1990 Volume 39 Issue 7 Pages 419-422
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAluminium readily reacts with DDAB (the title compound) in the presence of ethylenediamine (en) to form a stable fluorescent complex, which showed a maximum fluorescence intensity at pH values from 6.9 to 7.6. The fluorescence intensity of the complex increased remarkably with the addition of dioxane to its aqueous solution. The analytical procedure was as follows: Take 0?9 cm3 of a sample solution containing less than 3 μg of aluminium, and add 15 cm3 of a buffer solution described below and 1 cm3 of a 0.02% DDAB solution in dioxane. Dilute the mixture to 25 cm3 with water. After standing for 15 min, measure the fluorescence intensity at 575 nm with excitation wavelength of 485 nm by using 0.01?0.5 μg cm-3 of a Rhodamine B solution as the reference standard. When analysis of samples solution containing 0.005?0.05 μg of aluminium were required, 1 cm3 of a 0.004% DDAB solution was used. The buffer solution (pH 7.4) was prepared by adding 20 cm3 of en and 65 cm3 of (1+1) acetic acid to 200 cm3 of methanol and then diluting it to 500 cm3 with dioxane. The composition of the complex formed under the analytical conditions was Al:DDAB:en:acetate=1:1:2:1. En also acted as a masking agent of interfering ions. The proposed procedure was applied to the determination of aluminium in copper alloys.View full abstractDownload PDF (587K) -
Kuniaki KAWATA, Noboru MORIYAMA, Mitsugu KASAHARA, Yoshio URUSHIYAMA1990 Volume 39 Issue 7 Pages 423-425
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA simple sampling method using an activated carbon fiber paper was developed for GC determination of pesticides deposited on the ground in aerial application. The pesticides investigated were fenitrothion, malathion, tetrachlorvinphos and fenobucarb. Deposited pesticides were collected on a 5 cm×6 cm activated carbon fiber paper (Toyobo KF Paper P-175), and extracted ultrasonically with 3 ml of benzene-ethanol (4:1 v/v) for 10 min followed by centrifugation at 3000 rpm for 10 min. An aliquot of the supernatant was analyzed by GC on a 2 m×3 mm i. d. glass column packed with 5% silicone DC-200 on Chromosorb W AW-DMCS (60 to 80 mesh). Detectors used were FTD for fenobucarb and FPD for the other pesticides. The recoveries of the pesticides ranged from 88.2 to 102%. The minimum detectable amounts were 0.75 μg m-2 for fenitrothion, 1.5 μg m-2 for malathion, 2.6 μg m-2 for tetrachlorvinphos and 1.3μg m-2 for fenobucarb. Amounts of deposited pesticides measured by this method ranged from 11.4 to 151 mg m-2 within applied areas, and from 1.9 to 2900 μg m-2 in areas within 200 m from the boundary of aerial application.View full abstractDownload PDF (387K) -
Yushi SHICHI, Yasuhide INOUE, Masazi MATSUNAGA1990 Volume 39 Issue 7 Pages T93-T98
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA method was investigated for the determination and depth profile analysis of compounds of titanium, nitrogen and silicon using secondary ion mass spectrometry (SIMS). This was carried out using selected specific ions. Analytical conditions were as follows: primary ion: Cs+, 7 kV, 100 nA; measurement ion: positive ion. As the specific ions of titanium nitride, m/z 62, 110, 124 and 195 were chosen. They were derived from TiN, Ti2N, Ti2N2 and CsTiN, respectively. The specific ions of titanium silicide were m/z=76 and 104, which were derived TiSi and TiSi2. When this method was applied to the analysis of the joining interface, analytical results supported previous data obtained by XPS and AEM indicating that the joining interface of Si3N4-metal with active metal (Ti) and brazing metals (Ag/Cu) consisted of two layers.View full abstractDownload PDF (854K) -
Yumi TAKEUCHI, Shinichi WAKABAYASHI1990 Volume 39 Issue 7 Pages T99-T106
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSElemental analysis of a glassy phase at metallized alumina interface by ICP-AES following selective dissolution was studied. A test sample was prepared by printing tungsten paste on a green sheet (92% Al2O3-5.2% SiO2-2% MgO-0.8% CaCO3) and by sintering at 1570°C. The glassy phase formed was exposed by removing the metal layer by anodic stripping in 10% NaOH solution. Selective decomposition conditions for the glassy phase with sulfuric acid were studied using a Teflon pressurized decomposition vessel. The optimum decomposition was achieved at 200°C for 1.5 h with (1+5) sulfuric acid. In the ICP-AES determination, sulfuric acid reduced the emission intensities of Al, Si, Mg, Ca by approximately 10%. In order to compensate for the matrix effect, the use of a standard solution containing the same concentration of sulfuric acid as that in sample solution, 10 μg/ml of Al and Si, and 3 μg/ml of Mg and Ca was required. Variation of the total dissolved amount per sample was within 0.1 mg (n=5) and those of the chemical composition were ± 1% for Al2O3 and SiO2, ± 0.5% for MgO and CaO by the proposed method.View full abstractDownload PDF (5271K) -
Shigeru TANAKA, Katsutaka OKAMORI, Yoshikazu HASHIMOTO, Souichi SATO1990 Volume 39 Issue 7 Pages T107-T112
Published: July 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAttempts were made to determine low atomic number elements such as Al and Si in aerosols by XRF analysis. A simple method for correcting X-ray absorption effect for low atomic number element determination was investigated by using an intensity ratio between Compton and Thomson scattering. A linear relationship was found between mean atomic number (Z) of a sample and the scattering X-ray ratio (ICom/IThom), as follows.
ICom/IThom=-0.366Z+5.27(r=0.988)
The mean atomic munber (Z) of the aerosol sample was determined by measuring the scattering X-ray ratio (ICom/IThom). The mass attenuation coefficient (X) for the sample was then calculated from the mean atomic number (Z) and the measured wavelength (λ), as
X=C λ2.92Z3.07
Finally, the correction coefficient (t), which corrects the X-ray absorption effect, was calculated from the mass attenuation coefficient (X) and the aerosol mass weight (M), as
t=1-exp(-XMcosec 40)/XMcosec 40
Therefore, it is possible to correct the X-ray absorption effect by only measuring the scattering X-ray ratio. In order to evaluate this correction method, the same aerosol samples were analyzed by alkali fusion/ICP-AES. The corrected values of Al, Si and Ca obtained by XRF analysis agreed well with those by ICP-AES. Therefore, this correction method for the XRF analysis can be applied to the determination of low atomic number elements such as Al and Si in aerosols.View full abstractDownload PDF (920K)
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