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Volume 48, Issue 11
Displaying 1-9 of 9 articles from this issue
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Kiyokatsu JINNO, Hirokazu SAWADA1999 Volume 48 Issue 11 Pages 957-971
Published: November 05, 1999
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCapillary electrochromatography (CEC), which combines the advantages of high efficiency of capillary electrophoresis (CE) and high selectivity of liquid chromatography (LC), has recently received considerable attention. Most CEC experiments have been performed with capillary columns packed with small LC packing materials (1.5-5μm particle diameter). However, some problems, such as difficulties in packing the small LC packing materials and fabricating the frit, still exist in preparing the CEC column. The use of open-tubular columns in CEC is an alternative approach that eliminated such problems. So far, several types of open tubular columns have been reported for CEC separation.
In this review, recent progress in open-tubular columns for CEC is described.View full abstractDownload PDF (2801K) -
Hideo ASAKURA, Katsushige IKEGAMI, Hisanobu WAKITA1999 Volume 48 Issue 11 Pages 973-982
Published: November 05, 1999
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA glass-bead technique has been prepared under low temperature using a low flux-to-sample ratio molten mixture for the determination of the fluorine in calciumsilicate-fluoride composite materials by X-ray fluorescence spectrometry, because fluorides lose unnegligible amounts of fluorine at high temperature and the analytical line FKα for fluorine has low sensitivity. In the case of a 1: 1 flux(LiBO2)-to-sample, the test piece of this mixture began to contract at 640°C, became globular at 710°C and became transparent glass at over or around 760°C. A glass bead of a 1:1 flux-to-sample was successfully obtained by melting at 780°C for 10 minutes. Under these conditions, the reproducibility of the preparation of glass beads for samples containing artificial cryolite, which lost fluorine at high temperature, was found to be 0.154% as the relative standard deviation. In spite of the kinds of fluoride which were in the fluorine source, the samples could be homogenized by the glass-bead technique. The fluorine calibration equation can be regard as a CaO-CaF2 binary calibration according to the JIS correction model, making it possible to calculate the theoretical matrix correction coefficients(dj). The calibration also necessitated an overlapping correction for FeLα and MnLα. The fluorine calibration equation showed good precision, with 0.017 mass% as the standard deviation; it was possible to determine the fluorine from 0.2 to 12 mass% in many kinds of calciumsilicatefluoride composite materials.View full abstractDownload PDF (1697K) -
Motoyasu SUGIURA, Masao TSUJI, Atsushi MURASE, Takuya MITSUOKA1999 Volume 48 Issue 11 Pages 983-988
Published: November 05, 1999
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn analytic method, referred to as “derivatization/electron probe X-ray micro-analysis (EPMA)”, has been developed to determine the distribution of a small amount of carbonyl groups formed by the oxidation of polymers by chemical derivatization with 2, 4, 6-trichlorophenylhydrazine (TCPH). A suitable condition of the derivatization reaction with carbonyl groups in polymers was investigated. It was found that the highest reaction yield and selectivity were obtained by heating the sample in a 2.5% TCPH/acetic acid solution at 90°C for 30 min. Acetic acid was used as a catalyst and a solvent. By derivatization/EPMA using this reaction condition, a distribution measurement of the carbonyl group in the polymer became possible in 0.01% of the detection limits. Actual applications to a depth analysis of degraded ethylene-carbon mono oxide copolymer and polyethylene proved that this method is useful for the characterization of polymers and studies on polymer degradation.View full abstractDownload PDF (871K) -
Koichi YAMAMOTO, Noritsugu MATSUURA1999 Volume 48 Issue 11 Pages 989-998
Published: November 05, 1999
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the spectrophotometric determination of surfactants (cationic surfactants (CS+), such as quaternary ammonium salts, anionic surfactants (AS-), such as sodium lauryl sulfate and sodium alkyl sulfonate, and polyoxyethylene non-ionic surfactants (NS), containing a long-chain alkyl group) with Erythrosine B (EB), has been developed. The addition of CS+ to an EB solution buffered at pH 5.7 led to an increase in the absorbance at 549 nm; also, when AS- was added to the solution, the absorbance at 549 nm decreased with increasing the amount of AS-. This decrease in the absorbance was caused by an ion association of CS+ with AS-. A calibration graph based on this principle shows linearity up to 5 × 10-6 M of CS+ and AS- and from 10-6 to 10-4 order of NS. The proposed method is simple and rapid, and there is no use of toxic organic solvents. It was applied to the determination of anionic surfactants in commercial detergents for washing and kitchen, and cationic surfactants in commercial rinsing solutions for hair, the results of which were in good agreement with those of the JIS titration method (Epton method); also, it was applied to both the identification and the determination of non-ionic surfactants in commercial detergents for washing.View full abstractDownload PDF (1353K) -
Koji MATSUSAKI, Masanori NAGAHIRO, Toshikatsu SATA1999 Volume 48 Issue 11 Pages 999-1003
Published: November 05, 1999
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe surface of a gel-type anion exchange resin in the hydroxide form was modified by the adsorption of an anionic polyelectrolyte : a polycondensation product of sodium naphthalene sulfate and formaldehyde. After adsorption of the polymer, the rate of the ion-exchange reaction became slow. Especially, the ion-exchange rate of the sulfate ion was slower than that of the nitrate ion. Using the modified resin, in spite of the presence of the sulfate ion, the nitrate ion was preferentially adsorbed from the mixture solution of the nitrate and sulfate ions. The adsorbed ions were desorbed from the resin by use of potassium perchlorate or perchloric acid solutions. With these procedures, it was possible that the nitrate ion in the sulfate ion, the amount of which was 200-fold that of the nitrate ion, was separated and determined by ion-chromatography. The enrichment of nitrate ions to 50-fold its original concentration was also possible.View full abstractDownload PDF (814K) -
Motoyuki YAMAGAMI, Masahiro NONOGUCHI, Takashi YAMADA, Takashi SHOJI, ...1999 Volume 48 Issue 11 Pages 1005-1011
Published: November 05, 1999
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA combination of vapor-phase decomposition (VPD) and total reflection X-ray fluorescence (TXRF), VPD/TXRF, was used for measuring trace elements of Na and Al. A TXRF measurement using W-Mα line was carried out for a highly sensitivity analysis of ultra trace light elements. The technique of VPD/TXRF combining W-Mα excitation could clearly detect the peaks for a sample at a level of 1011 atoms cm-2 that conventional TXRF could not have detected. In the case of 150 mm Si wafers, the lower limits of detection (LLDs) were found to be 3 × 1010 atoms cm-2 and 2 × 109 atoms cm-2 for Na and Al, respectively. The LLDs were improved by two orders of magnitude compared with those of TXRF without using the VPD treatment. The results obtained by VPD/TXRF were cross-checked with the one obtained by AAS. Both values were in good agreement. The glancing-angle dependence of the TXRF intensity was investigated on the samples before and after undergoing the VPD treatment. This dependence proves that the sample after a VPD treatment is the particle type on the wafer.View full abstractDownload PDF (1199K) -
Yuka EZOE, Akiko TAKATSU, Takayoshi KUROIWA, Sakae EYAMA, Akira UCHIUM ...1999 Volume 48 Issue 11 Pages 1013-1018
Published: November 05, 1999
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of trace levels of Al in biological materials (fish) by graphite-furnace AAS was studied. Samples were digested with HNO3, since HClO4 gave great interferences to the determination of Al. The analytical wavelength was selected at 394.4 nm, and the ashing and atomizing temperatures were fixed at 1500°C and 2600°C, respectively. Interferences of coexisting inorganic components (Ca, Na, K, Mg, Fe and P) were also studied. The torelable concentrations for respective components were as follows: Ca 500 mg dm -3, Na 50 mg dm -3, K 50 mg dm -3, Mg 100 mg dm -3, Fe 20 mg dm -3 and P 200 mg dm -3. Prior to the Al analysis, samples should be diluted with water in order that the concentration of each inorganic component be lower than that mentioned above. In all standard and sample solutions the concentration of HNO3 were maintained in 0.1% (v/v). The Al concentrations in biological reference materials (NRCC DORM-2 and DOLT-2) determined by the present method agreed well with the reported reference values. The detection limit (3δ) was 1 ng g-1 (dry weight of biological samples). The present method is applicable with high accuracy and sensitivity to the determination of Al in biological samples.View full abstractDownload PDF (915K) -
Kazuko YAMAMOTO, Hideyuki SAKAMOTO, Masako NISHIMURA, Akira YONETANI, ...1999 Volume 48 Issue 11 Pages 1019-1022
Published: November 05, 1999
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA chemical modifier was studied to analyze selenium in enteral formulas and urine samples using graphite-furnace AAS. Pd(1000 mg/l) + Mg(1000 mg/l) + citric acid (20%) was proper for the chemical modifier. NIST SRM 1549 (Non-Fat Milk Powder) and NIST SRM 2670 (Toxic Metals in Freeze-Dried Urine) were analyzed by this method; the results met the guaranteed values within the range of the analytical error. The detection limit (concentration corresponding to 3σ of the absorbance of the blank) by this method was 0.32 μg/l, and the repeatability of the absorbance with a concentration of 20 μg/l was 2% (n=5).View full abstractDownload PDF (504K) -
Hiroto OZAKI, Yoshihide TANAKA, Shiro MATSUOKA, Kazuko MIZUISHI1999 Volume 48 Issue 11 Pages 1023-1030
Published: November 05, 1999
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1434K)
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