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Volume 44, Issue 3
Displaying 1-14 of 14 articles from this issue
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Simple methods for preconcentration of trace elements in waterKatsumi GOTO, Noriko HATA1995 Volume 44 Issue 3 Pages 169-180
Published: March 05, 1995
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSimple methods for preconcentration and determination of trace elements in water are reviewed in some detail. The topics selected are
1. Measurement of absorbance or reflectance of a solid phase in which trace analytes are collected as colored species.
2. Visual and photometric determination after enrichment onto a transparent film as colored species.
3. Enrichment with solvent-soluble filters.
4. Enrichment exploiting temperature- and polymer-induced separation of a micelle-rich phase from homogeneous solution.
5. Concentration into one drop of water-miscible solvent.
6. Determination by graphite furnace atomic absorption spectrometry after separation as a gas and in-situ concentration in a graphite furnace.View full abstractDownload PDF (2260K) -
Haruo IWABUCHI, Eiichi KITAZAWA, Akihiko NAKAGAWA, Kan-ichi NAKAMURA1995 Volume 44 Issue 3 Pages 181-188
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn this study a column switching system was introduced between the LC/atmospheric pressure chemical ionization (APCI)-MS interface and HPLC. This method introduced only the objective components to MS without the need for troublesome pretreatment to remove contaminants from biological samples, effectively cleaning the interface and modifying the analytical conditions. After addition to rat plasma, drugs and their polar metabolites were analyzed simultaneously and identified. The metabolites were detected after administration of the drugs to rats, and their structures were elucidated. Further, we have clarified some characteristic aspects of the LC/APCI-MS interface.View full abstractDownload PDF (1076K) -
Tsunemi AIBA, Kin-ichi TSUNODA, Hideo AKAIWA1995 Volume 44 Issue 3 Pages 189-194
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSOne of the disadvantages of a synergistic extraction is that the addition of a synergist usually decreases the selectivity for a particular metal ion in the extractive separation. However, the addition of the synergist to a chelate extraction system may increase the number of factors controlling the selectivity. Thus, synergistic extraction system with mixed additives (1, 10-phenanthroline=phen and pyridine=py/4-methyl-pyridine=4-me-py) was adopted, aiming to improve mutual separation of their ions. When 1, 1, 1-trifluoro-4-mercapto-4-(2-thieny1)-3-butene-2-one (STTA) was used as the chelating agent, the addition of mixed additives, phen and py or 4-me-py, increased the extractability of CdII compared with the addition of a single additive. In particular, the effect of phen and 4-me-py was remarkable. On the other hand, no such effect was observed in ZnII extraction. Hence, the degree of mutual separation between CdII and ZnII was improved by the addition of the mixed neutral ligands.View full abstractDownload PDF (770K) -
Matashige OYABU, Yoshinori KOBAYASHI, Tadao SEGUCHI, Tsuneo SASUGA, Hi ...1995 Volume 44 Issue 3 Pages 195-201
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSOrganic polymers used in atomic power plants or space are damaged by ionizing irradiation. Radicals produced by irradiation cause oxidation, chain scission and crosslinking, all of which lead to degradation of the material. In this paper, the surface of electron-irradiated poly-ether ether ketone (PEEK) was studied by X-ray photoelectron spectroscopy (XPS). The irradiation in air was found to oxidize the PEEK surface producing carboxyl groups, the content of which dependant on the dose. Carboxyl groups were not produced in helium gas. Quantitative spectral analysis indicated that the aromatic structure might be decomposed. Some comparison was made between the semicrystalline and amorphous samples. The oxygen content resulting from irradiation, of semicrystalline PEEK increased more than that of amorphous PEEK.View full abstractDownload PDF (959K) -
Yoshinori INOUE, Katsuhiko KAWABATA, Hiromitsu TAKAHASHI, Ginji ENDO1995 Volume 44 Issue 3 Pages 203-208
Published: March 05, 1995
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSInorganic and organic arsenic compounds, i.e. arsenic acid (AsV), arsenous acid (AsIII), monomethylarsonic acid (MMAs), dimethylarsinic acid (DMAs), trimethylarsine oxide (TMAsO) and arsenobetaine (AsBe), were analyzed by a combined system of inductively coupled plasma mass spectrometry with ion chromatography (IC/ICP-MS). The arsenic compounds were separated by ion exclusion chromatography, size exclusion chromatography and anion exchange chromatography. Subsequently eluates were directly introduced into ICP-MS and detected at m/z=75. The six arsenic compounds were completely separated by ion exchange chromatography. Separation parameters were optimized for the arsenic compounds as follows: column, Excelpak ICS-A35×2 (150 mm×4.6 mm i.d.×2) packed with hydrophilic polymer based anion exchange resin; mobile phase, 0.01 mol l-1 tartaric acid; flow rate, 1.0 ml min-1; injection volume, 20 μl. The detection limits for the arsenic compounds were from 0.22 to 0.44 μl l-1 (from 4.4 to 8.8 pg) as As element. The reproducibility (n=5) was better than 5% of the relative standard deviation (RSD) for the arsenic compounds.View full abstractDownload PDF (1095K) -
Shogo SUZUKI, Shoji HIRAI1995 Volume 44 Issue 3 Pages 209-215
Published: March 05, 1995
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSTrace elements in high grade pure iron certified reference materials (JSS001-3, JSS001-4) and iron ore certified reference materials (JSS803-4, JSS805-1) prepared by the Iron and Steel Institute of Japan were determined by instrumental neutron activation analysis (INAA). The high grade pure iron samples (ca. 130750 mg) and iron ore samples (ca. 140290 mg) were irradiated for 2 min at a thermal neutron flux of 1.5×1012 n cm-2 s-1 and for 6 h at a thermal neutron flux of 3.7×1012 n cm-2 s-1 in the Rikkyo University Research Reactor. Conventional γ-ray spectrometry with a coaxial Ge detector and anti-coincidence γ-ray spectrometry with a coaxial Ge detector and a well-type NaI(T1) detector were used for γ-ray counting. The irradiated samples were measured at very high count-rates in the γ-ray spectrometries, because of the strong radioactivity from the matrix element. A pulse pile-up rejector was used in both γ-ray spectrometries in order to correct for counting loss. For the high grade pure iron certified reference materials, the concentration of 8 elements (Al, Cl, V, Co, Cu, As, Zn, W) in JSS001-3 and 8 elements (Na, Al, Cl, V, Co, As, Zn, W) in JSS001-4 were determined by these methods. The concentration of 2933 elements in the iron ore certified reference materials (JSS803-4, JSS805-1) were determined. The determined values were in good agreement with the certified and reference values.View full abstractDownload PDF (1003K) -
Tadashi MIYAZAWA, Kunio NAKAJIMA, Yukio MINAMI, Hiroshi UCHIHARA, Masa ...1995 Volume 44 Issue 3 Pages 217-219
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe pinpoint condensation technique using perfluorated polymer film was applied to the identification of tetrahydrocannabinol (THC), the primary psychoactive constituent of marijuana. Rapid solvent elimination for condensation of THC into a small single residual at room temperature was performed by solvent evaporation on perfluorated polymer film, and the residual was measured by the microscope/FTIR technique. This sample condensation method provided high sensitivity for IR analysis. The detection limit was at the subnanogram level, and the sensitivity was nearly equal to that of gas chromatography using a mass spectrometer.View full abstractDownload PDF (507K) -
Masaaki TABATA, Shinobu KODA, Keiji YASUDA, Hiroyasu NOMURA1995 Volume 44 Issue 3 Pages 221-225
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe reaction of lead(II) and zinc(II) with 5, 10, 15, 20-tetrakis(4-sulonatophenyl)-porphyrin (H2tpps4-) was studied under ultrasonic irradiation at 20 kHz and 40 kHz to clarify the effect of ultrasonic irradiation on metalloporphyrin formation. The power intensities of the ultrasonic irradiator, given in terms of the concentration of nitric acid generated during ultrasonic irradiation, were 2.66×10-5 M h-1 and 1.05×10-5 M h-1 for 20 kHz and 40 kHz, respectively. Temperature was strictly controlled during the ultrasonic irradiation. The ultrasonic irradiation caused the metalloporphyrin formation to slow down and led to the decomposition of the metalloporphyrin rather than the acceleration of the metalloporphyrin formation. The ultrasonic irradiation-induced decomposition of H2tpps4-, Pb(tpps)4- or Zn(tpps)4- was more effective at 20 kHz than 40 kHz. The decomposition rate of the porphyrins increased in the order H2tpps4-≤Zn(tpps)4-≤Pb(tpps)4-. Ninety-four percent of lead(II) porphyrin was decomposed by ultrasonic irradiation for 60 min at 20 kHz.View full abstractDownload PDF (782K) -
Buffer solutions for capillary electrophoresis using the formation of saccharideboric acid complexesMichio ZENKI, Masaru IRIZAWA, Hidenori YUKUTAKE1995 Volume 44 Issue 3 Pages 227-229
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe pH of electrophoretic buffer solutions is an important factor affecting the separation of analytical species by capillary electrophoresis. In pH adjustment, the use of electrolytes increases the ionic strength. The increased current against the high voltage (≥10 kV) generates Joule heat and ruins the separation. Thus it is necessary to prepare buffer solutions without increasing ionic strength. The saccharide-borax system was found to be suitable for this purpose. Saccharide reacts with boric acid to form a dissociable complex, the pH varying from 4 to 9 easily. In this experiment, fructose was used as the saccharide and ten aminonaphthalenesulfonic acids (ANS) were selected as model compounds for separation. The pH dropped as fructose was added. By adding 600 mM fructose in 20 mM borax solution (pH 4.6), nine ANS were separated successfully.View full abstractDownload PDF (346K) -
Akiyo(nee Motoyama) MIZUTANI, Masamichi YOSHIDA1995 Volume 44 Issue 3 Pages 231-235
Published: March 05, 1995
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe determination of silicon in positive type photoresist was studied using graphitefurnace Zeeman-type AAS by preconditioning the furnace with calcium. Calcium solution in 0.02 M HCl injected into the furnace before the sample injection enhanced silicon absorbance by 50%. The wavelength, band width and current of the silicon hollow cathode lamp were 251.6 nm, 0.4 nm and 10 mA, respectively. The solutions were injected into the furnace in the following order: calcium solution (drying at 120°C and ashing to 550°C), silicon standard solution (with standard addition method, drying at 120°C), and diluted photoresist. The optimum furnace program determined for silicon consisted of drying for 10 s at 150°C (ramp mode), first ashing for 15 s to 850°C (ramp mode), second ashing for 25 s to 1200°C (ramp mode), atomizing for 10 s at 2800°C (flash mode) and cleaning for 3 s at 3000°C (step mode). The detection limit of silicon by the in-furnace standard addition was found to be 0.02 ng and the relative standard deviation for photoresist (n=5) was 5%.View full abstractDownload PDF (680K) -
Hiroshi KAWAMOTO, Hideyuki ITABASHI, Tomoyuki OHNUKI1995 Volume 44 Issue 3 Pages 237-240
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSOn the basis of the HSAB principle, a method for extraction of metal ions with diethyldithiocarbamic acid (DDTC) consisting of the preconcentration and separation of trace metal ions was developed. Metal ions extracted into CCl4 were back-extracted into Cu-EDTA solution which was applied to isotachophoretic analysis. This method made possible the separation of CdII, FeII, PbII and ZnII at 10-6 mol dm-3 level.View full abstractDownload PDF (489K) -
Yasuaki TAKADA, Motoko YOSHIDA, Minoru SAKAIRI, Hideaki KOIZUMI1995 Volume 44 Issue 3 Pages 241-246
Published: March 05, 1995
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSubstances related to brain function (neurotransmitters and brain peptides) were analyzed by capillary electrophoresis/mass spectrometry (CE/MS). An ammonium acetate buffer, commonly used for CE/MS with an electrospray interface, was used to separate the substances. Micellar electrokinetic capillary chromatography/mass spectrometry was also used to analyze catecholamines (Dopamine, Epinephrine, Norepinephrine). The detection limits were about 100 fmol for catecholamines, 10 fmol for some other substances (GABA, uridine and glutathione), and 0.11 fmol for brain peptides, when using a 50 μm i.d. analytical capillary column. We believe CE/MS will be a useful technique for analyzing brain substances, because of its characteristics of high separation efficiency, small sample consumption, and high identification ability.View full abstractDownload PDF (776K) -
Yasuhiko NISHIKAWA, Jun'ichiro MIURA1995 Volume 44 Issue 3 Pages 247-250
Published: March 05, 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDownload PDF (827K) -
1995 Volume 44 Issue 3 Pages e1
Published: 1995
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDownload PDF (72K)
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