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Totaro IMASAKA
1993 Volume 9 Issue 3 Pages
329-344
Published: June 10, 1993
Released on J-STAGE: July 04, 2006
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A semiconductor laser is more compact and less expensive than a conventional laser. Therefore, scientists prefer to use this light source in analytical spectroscopy. However, the emitting wavelength of the semiconductor laser is located in the near-infrared or deep-red region. Only a limited number of compounds are fluorescent in these spectral regions; we have already developed many analytical reagents and procedures for application. Inorganic species such as potassium ions and oxygen gas, organic molecules such as dyes and surfactants, and biological molecules such as metabolites, enzymes, proteins, and deoxyribonucleic acid have been determined by this method. For example, amino acids are determined at zeptomole levels after labeling them with a dye fluorescent in the deep-red region and separation by capillary electrophoresis. Thus semiconductor laser spectrometry is advantageous for practical trace analysis.
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Tohru SAITOH, Hirofumi TANI, Tamio KAMIDATE, Hiroto WATANABE, Kensaku ...
1993 Volume 9 Issue 3 Pages
345-349
Published: June 10, 1993
Released on J-STAGE: July 04, 2006
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The aggregation number of
N-octanoyl-
N-phenylhydroxylamine (C8-PHA) in carbon tetrachloride was determined on the basis of the extraction equilibria of copper(II) chelate with C8-PHA between aqueous and carbon tetrachloride phases. According to the relation of the distribution ratio of copper(II) with its concentration in the organic phase, the formation of a reversed micelle consisting of approximately 13 C8-PHA molecules was deduced when C8-PHA concentration was greater than 0.1mol dm
-3. The Karl Fisher titration results showed that one water molecule was included in the reversed micelle. The polar parameter (
ET(1)) of the reversed micelle was determined to be 250kJ mol
-1 by measuring absorption spectra of 1-(4-hydroxyphenyl)-2, 4, 6-triphenylpyridinium betaine (HPTPP) as a function of C8-PHA concentration in carbon tetrachloride. The
ET(1) value was different from that in carbon tetrachloride, indicating the incorporation of HPTPP into the polar core region where the hydrophilic chelating groups are oriented inward in the reversed micelle. On the basis of the
ET(1) values in organic solvents, the polar core region could be regarded as being an alcoholic medium.
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Hirofumi SUZUKI, Hiroshi NAKAGAWA, Masaki MIFUNE, Yutaka SAITO
1993 Volume 9 Issue 3 Pages
351-354
Published: June 10, 1993
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A new sensitive and selective electrode for triiodide ion has been developed. The electrode was constructed by incorporating Mn(III)-tetraphenylporphine into a plasticized poly(vinyl chloride) membrane. The electrode shows super-Nernstian response over the range 10
-5 to 10
-3M triiodide ion in the pH range of 2 to 9, with an anionic slope of 87 mV/ concentration decade. The electrode exhibits high specificity for triiodide ion over other anions (salicylate, benzoate, propionate, perchlorate, iodide, bromide, chloride, fluoride, nitrate and bicarbonate). The electrode has been applied to measure triiodide ion generated from iodine. The results have indicated that iodine can be determined by simple potentiometric measurements. A similar method may be applied to determine oxidizing agents, bromine and hydrogen peroxide, which oxidize iodide ion to iodine.
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Hisanori IMURA, Hideyuki IKEDA, Kayoko NAKAYAMA, Kousaburo OHASHI
1993 Volume 9 Issue 3 Pages
355-359
Published: June 10, 1993
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The extraction behavior of Mn
II, Fe
III, Co
II, Ni
II, Cu
II, Zn
II, Ga
III, and Cd
II was studied with a new chelating extractant, 5-(4-nitrophenylazo)-7-(4-ethyl-1-methyloctyl)-8-quinolinol (HNEQ), in chloroform. HNEQ exhibits a much higher extractability for Co
II, Cu
II, Zn
II, and Cd
II than 8-quinolinol. Especially, Cu
II was quantitatively extracted with 0.001mol dm
-3 of HNEQ at such a low pH as 2.0 within 15min, and was readily separated from the other metal(II, III) ions studied. From equilibrium studies, the extracted Cu
II-HNEQ chelate was ascertained to be Cu(NEQ)
2. The extraction constant (log
Kex) was determined to be 4.25, which was much larger than those for 7-(4-ethyl-1-methyloctyl)-8-quinolinol (Kelex 100) and 8-quinolinol.
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Tatsuya SEKINE, Nguyen THI KIM DUNG
1993 Volume 9 Issue 3 Pages
361-366
Published: June 10, 1993
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Cerium(III) in aqueous 0.1mol dm
-3 sodium nitrate solutions was extracted with benzoyltrifluoroacetone (Hbfa) into carbon tetrachloride in the absence and presence of tetrabutylammonium (tba
+). In the absence of tba+, only the Ce(bfa)
3 was extracted; in its presence, however, not only was the ternary complex (Ce(bfa)
4-tba
+) also extracted, and the extraction was much better. When the two-phase agitation was continued, the organic phase gradually changed from colorless to brown in the absence of tba
+ due to the oxidation of the metal ions in the complex in the organic phase to the cerium(IV). However, in the presence of tba
+, the organic phase remained colorless for a long time and, thus, oxidation of the cerium(III) was negligible. The rate of oxidation of cerium(III) in the Ce(bfa)
3 complex in carbon tetrachloride to the cerium(IV) by forming the Ce(bfa)
4 complex was measured by spectrophotometry. The rate of this oxidation was found not to be affected by the ligand concentration.
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Masataka HIRAIDE, Naoki OZAKI, Yong-Nam PAK, Tomokazu TANAKA, Hiroshi ...
1993 Volume 9 Issue 3 Pages
367-370
Published: June 10, 1993
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In a stream (5ml min
-1) of water sample, traces of copper(II) ions are quantitatively coprecipitated with indium hydroxide and floated with the aid of anionic surfactants and nitrogen bubbles. The precipitate-foam layer is continuously dissolved in 4mol l
-1 nitric acid and collected at intervals. The copper is concentrated 25-fold and determined by inductively coupled plasma-atomic emission spectrometry. The indium carrier is also determined to obtain the copper/indium intensity ratios. The coprecipitation-flotation in a flow system responds well to the changes of copper concentrations.
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Catherine FAVEN, Marc DEBACKER, Didier BARBRY
1993 Volume 9 Issue 3 Pages
371-374
Published: June 10, 1993
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A simple and rapid chemiluminescent method has been developed for the assay of benzoyl peroxide in organic or aqueous solvents. Some nitrogen reagents were tested regarding their ability to produce chemiluminescence by reacting with benzoyl peroxide. Triethylamine and quinuclidine have been found to be suitable amines for this method. The products of the reaction were confirmed by nuclear magnetic resonance spectroscopy. Other primary or secondary amines or amides also produce a chemiluminescent reaction with Benzoyl peroxide, although the intensity of the luminescence is smaller. 9, 10-Dibromoanthracene, pyrene or rubrene are effective enhancers of the chemiluminescent reactions examined. Ten ng/ml of benzoyl peroxide in chloroform can be detected using triethylamine and rubrene as chemiluminescent reagents. Therefore, the limit of benzoyl peroxide detection has been lowered by a factor of about 2000. The presence of the aromatic compound probably induces an energy transfer which helps in the formation of excited states on this molecule.
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Masahiko HIRANO, Yutaka YAMASHITA, Atsuo MIYAKAWA
1993 Volume 9 Issue 3 Pages
375-380
Published: June 10, 1993
Released on J-STAGE: July 04, 2006
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A new type of video-microscope system combined with a fiber-optic plate processed in the shape of a needle has been developed; the obtained fluorescence images were analyzed. The fiber-optic plate comprises thousands of optical fibers 3μm in diameter, a sufficient size for viewing a single cell. Images at areas adjacent to the end of the fiber-optic plate are transmitted into an objective and detected with a video camera. They are then digitized for storage in an image processor. Using this system and fluorometric methods, cultured cells can be sufficiently visualized and any spatiotemporal change in the intracellular free calcium concentration can be measured. These specifications suggest that the activity and morphology of cells in internal parts of a living animal can be measured at the single-cell level by inserting a fiber-optic plate into the target organ.
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Koji MATSUSAKI, Tsutomu OISHI
1993 Volume 9 Issue 3 Pages
381-384
Published: June 10, 1993
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A mixture of ammonium-EDTA, nickel and copper nitrates is suitable as a matrix modifier for the removal of sulfate interference in the determination of bismuth by graphite furnace atomic absorption spectrometry. A mixture of ammonium-EDTA and nickel nitrate is suitable as the modifier for a thallium determination. In the presence of sodium sulfate, the tolerable ashing temperatures for bismuth and thallium were decreased. Although an organic compound, such as EDTA, enhances the interference from sulfate, by the addition of nickel and copper nitrates this interference can be removed. Since analyte and other cations are masked by EDTA, the coexisting sulfates are converted to ammonium salt, which is readily decomposed and eliminated from the furnace during the ashing step. In the presence of these matrix modifiers, the tolerable concentrations of coexisting sodium sulfate for bismuth and thallium were
ca. 1000-times greater than those in the absence of the modifier.
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Kei YAMADA, Osamu KUJIRAI, Ryosuke HASEGAWA
1993 Volume 9 Issue 3 Pages
385-390
Published: June 10, 1993
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Boron, Mo, Nb, Sn, Ta, W and Zr were separated from an iron matrix using a horizontal mini-column of an anion exchange resin. The flow of solutions through the mini-column was controlled by a peristaltic pump. The elements adsorbed on the resin were simultaneously eluted by the circulation of an eluant and determined by inductively coupled plasma-atomic emission spectrometry. Quantitative recoveries were obtained for all 7 elements in the acid-soluble fraction and for 5 elements (not B or Sn) in the acid-insoluble fraction. A part of B in the acid-insoluble fraction was lost during the ashing and the fusion but the loss was compensated by using the calibration solutions prepared with the same procedure as that for the samples. A 500-fold enrichment was obtained using this preconcentration system compared with an ordinary sample solution of 0.5g/100cm
3. The proposed method was applied to the simultaneous determination of sub μg g
-1 levels of impurities in high purity irons.
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Yoshio IIDA, Shigeki DAISHIMA, Fujihiro KANDA
1993 Volume 9 Issue 3 Pages
391-395
Published: June 10, 1993
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A probe-type insertion discharge electrode for Townsend discharge chemical ionization, which offers characteristic ionization, was developed to fit commercially available mass spectrometers. Studies on reactant ions formed from reagent gases (O
2, NO, CH
4) showed that the position of the electrode in the ion source, its insulation, and the applied voltage were of particular importance. Elements such as material, diameter and shape of the electrode were found to be of less significance. Mass spectra and peak profiles obtained by selected ion monitoring of standard compounds showed this probe-type electrode to be of practical value.
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Yoshihiko IKEGUCHI, Hiroshi NAKAMURA, Terumi NAKAJIMA
1993 Volume 9 Issue 3 Pages
397-399
Published: June 10, 1993
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Flow injection analysis (FIA) was applied to the determination of organic phosphates such as phosphoamino acids and nucleotides. Under the optimized condition, organic phosphates were heated in a hydrolysis coil at 170°C in 2.0Msulfuric acid for 5.8min, most of organic phosphates being hydrolyzed at the rate of over 80%. The resultant orthophosphate was monitored at 830nm after the selective reaction with a molybdenum reagent. When 50μM O-phospho-DL-tyrosine solution was employed (injection volume: 5μl), the present FIA method enabled the analysis of 20 samples h
-1 with a relative standard deviation of 2.6% (
n=20). The detection limits (
S/N=2) of organic phosphates were
ca. 50pmol. The present FIA system is expected to be useful as a postcolumn reaction detector for high-performance liquid chromatography of organic phosphates.
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Tomoaki ARIMURA, Masaaki SHIBATA, Hirotaka IHARA, Chuichi HIRAYAMA
1993 Volume 9 Issue 3 Pages
401-403
Published: 1993
Released on J-STAGE: July 27, 2007
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Erkang WANG, Zemu Yu, Chengmin Xu, Deyao QI
1993 Volume 9 Issue 3 Pages
405-408
Published: June 10, 1993
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Anu WAHI, L. R. KAKKAR
1993 Volume 9 Issue 3 Pages
409-413
Published: June 10, 1993
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Tsunehiko OTOSHI, Yasumi IZUMIKAWA, Osamu INO
1993 Volume 9 Issue 3 Pages
415-417
Published: June 10, 1993
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Kazuichi HAYAKAWA, Jun KOBAYASHI, Mikako OHMORI, Mayumi OHYA, Akio KAT ...
1993 Volume 9 Issue 3 Pages
419-421
Published: June 10, 1993
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Koji YAMAGAKI, Michinao YOSHII, Keio YAMADA
1993 Volume 9 Issue 3 Pages
423-424
Published: June 10, 1993
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Masao BOUNOSHITA, Kiyokatsu HIBI, Hiroshi NAKAMURA
1993 Volume 9 Issue 3 Pages
425-428
Published: June 10, 1993
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C. L. CHEN, J. D. RODER, S. SANGIAH, H. CHEN, K. D. BERLIN, G. L. GARR ...
1993 Volume 9 Issue 3 Pages
429-431
Published: June 10, 1993
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Crystal Structure of (5RS, 6RS, 1ORS, 11RS)-5, 6, 10, 11-Tetrahydro-5-acetyl-8-formyl-10-hydroxy-4, 11-dimethoxy-7, 7, 9-trimethyl-6, 10-methano-7H-benzocyclononene
Yuko KOJIMA, Yasuko T. OSANO, Takao MATSUZAKI, Yoshiaki HORIGUCH, Isao ...
1993 Volume 9 Issue 3 Pages
433-434
Published: June 10, 1993
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Yasuo WAKATSUKI, Reiko SHIMADA, Yasuhiro YAMAMOTO, Hiroshi YAMAZAKI
1993 Volume 9 Issue 3 Pages
435-436
Published: June 10, 1993
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Yoshiharu NAWATA, Masahiro KATO, Kiyoshige OCHI, Masafumi FUKUSHIMA
1993 Volume 9 Issue 3 Pages
437-438
Published: June 10, 1993
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Manuel SORIANO-GARCIA, René Villena IRIBE, Adrian COVARRUBIAS, ...
1993 Volume 9 Issue 3 Pages
439-440
Published: June 10, 1993
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Yasuko T. OSANO, Kaoru HORIUCHI, Jun-ichi MATSUURA, Takao MATSUZAKI
1993 Volume 9 Issue 3 Pages
441-442
Published: June 10, 1993
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