Analytical Sciences
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Volume 3, Issue 6
Displaying 1-26 of 26 articles from this issue
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  • 36th Annual Meeting of The Japan Society for Analytical Chemistry
    Shujiro GOYA
    1987 Volume 3 Issue 6 Pages 477
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.477
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  • Second Japan-Korea Joint Symposium on Analytical Chemistry
    Yosuke OHKURA
    1987 Volume 3 Issue 6 Pages 478
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.478
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  • Ion-Association Reagents A Review1
    Kyoji TOEI
    1987 Volume 3 Issue 6 Pages 479-488
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.479
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    Ion-association reagents are widely used for analytical chemistry. The ion-associable cation or anion should be univalent, bulky and charge-dispersed. The reagents are classified by their shape: plane, sphere, chain and polymer types. The ion-associable cation and anion can combine with each other to form the ion-associate in water. This phenomenon has been used for gravimetric and volumetric analyses and for extraction-spectrophotometry of a trace component. Several examples of specific and sensitive extraction-spectrophotometries are illustrated. The polymer type reagent can react with the counter-charged poly-electrolyte to form a precipitate quantitatively, and it can be used for colloid titration. Metachromasy phenomenon is based on the formation of the ion-associate of colored ion-associable cation or anion with counter-charged colorless ion-association reagents to show distinguished color changes.
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  • Chloride Isolation for Accelerator Mass Spectrometry of 36Cl Produced by Atomic Bomb Neutrons
    Kazuo KATO, Manabu YAMAMOTO, Masayoshi NONAKA, Takahiro KUMAMARU, Yuro ...
    1987 Volume 3 Issue 6 Pages 489-491
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.489
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    Accelerator mass spectrometry was performed at the Munich tandem laboratory to determine the ratio of 36Cl/Cl in silicate rock samples exposed to neutrons of the Hiroshima atomic bomb. Chloride was chemically separated from silicate rock for this purpose. Five grams of silicate rock was fused with 30g of sodium hydroxide and dissolved in 900ml of water. The chloride in the resulting solution was spectrophotometrically determined. Chloride was precipitated as silver chloride by addition of appropriate amounts of silver nitrate, and silver chloride was then collected on a membrane filter. The chloride in the rock samples was thus isolated quantitatively.
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  • Europium Isolation from Silicate Rock Samples Exposed to Hiroshima Atomic Bomb Neutrons
    Kazuo KATO, Manabu YAMAMOTO, Takahiro KUMAMARU, Yuroku YAMAMOTO, Minor ...
    1987 Volume 3 Issue 6 Pages 493-497
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.493
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    A method was devised for isolating europium from silicate rock samples, and was applied to the measurement of gamma-rays from 152Eu in silicate rocks exposed to the Hiroshima atomic bomb. Rock samples were powdered and fused with sodium hydroxide. A cation exchange separation technique was used to separate europium from the foreign ions. The amount of europium isolated was determined by electrothermal atomic absorption spectrophotometry.
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  • Supporting Electrolytes for Voltammetric Study of Ion Transfer at Nitrobenzene/Water Interface
    Toshiyuki OSAKAI, Tadaaki KAKUTANI, Yoshinori NISHIWAKI, Mitsugi SENDA
    1987 Volume 3 Issue 6 Pages 499-503
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.499
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    The polarizable potential range was determined by cyclic voltammetry for the interface between an aqueous solution of lithium chloride or magnesium sulfate and a nitrobenzene solution of various electrolytes: tetrabutylammonium salts of tetraphenylborate, tetrakis(4-fluorophenyl)borate, tetrakis(4-chlorophenyl)borate, and tetrakis[3, 5- bis(trifluoromethyl)phenyl]borate, and tetrapentyl- and tetrahexylammonium salts of tetraphenylborate. The anodic and cathodic limits of polarizable potential range were discussed with reference to the standard ion-transfer potentials of the supporting-electrolyte ions.
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  • Molecular Structure and Extraction Behavior of Silver(I)-13, 14-Benzo- 1, 4, 8, 11-tetrathiacyclopentadec-l3-ene Picrate Complex
    Eiichi SEKIDO, Kohei SUZUKI, Kensaku HAMADA
    1987 Volume 3 Issue 6 Pages 505-508
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.505
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    The X-ray crystallographic analysis of silver(I)-13, 14-benzo-1, 4, 8, 11-tetrathiacyclopentadec-l3-ene picrate (Ag-Bz- TTCP-Pic) was carried out. The molecular structure of its complex cation is discussed in connection with its solvent extraction behavior. The Ag-Bz-TTCP cation complex is not the simple 1:1 monomer complex cation, [Ag(bz-ttcp)]+, but the 2:2 dimeric complex cation, [Ag2(bz-ttcp)2]2+. Each silver(I) ion has the coordination number 5 and binds with five sulfur atoms: four sulfur atoms in one Bz-TTCP molecule and one sulfur atom in another Bz-TTCP, to form a distorted square pyramidal configuration. Thus two silver(I) ions are sandwiched between two Bz-TTCP molecules so that they look as if they were surrounded with two cyclic polythioether rings and two benzene rings. The charge on two silver(I) ions is delocalized on the dimeric complex. Thus the formation of the ion pair complex with two picrate anions is so stabilized that silver(I) will be almost completely extracted.
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  • Interactions of Solid Supports and Fluorescent Substances in Thermally Activated Delayed Fluorescence
    Yoshiaki ONOUE, Keizo HIRAKI, Yasuharu NISHIKAWA
    1987 Volume 3 Issue 6 Pages 509-513
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.509
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    The effect of the solid support on thermally activated delayed fluorescece (TADF) was investigated. Comparison of the molecular structures of supports and consideration of the energy levels of the absorption band and the fluorescence, and of lifetimes of emissions allowed the postulation of certain molecular criteria for the supports of TADF. The interactions of Tin-protoporphyrin IX dimethyl ester (Sn-PPDE) with a polyvinyl alcohol (PVA) were considered in detail. The hydrogen bonds (-OH-π-electron systems of Sn-PPDE) were found to contribute to fix Sn-PPDE rigidly in the PVA matrix, thereby minimizing non-radiative decay of the excited molecule in the triplet state.
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  • Errors in Acid-Base Titration Using Gran′s Plot Method
    Naoshige AKIMOTO, Hisako HANAKUMA, Keiichiro HOZUMI
    1987 Volume 3 Issue 6 Pages 515-519
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.515
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    A statistical end point error in the strong acid-strong base titration using the Gran′s plot method has been studied theoretically on the basis of an individual source of errors arising in the course of determination. Errors in potential reading of the electrode system and in temperature reading of the titration solution were evaluated by the standard deviation of the volume at the end point as a function of the mean titration fraction of the data points used for extrapolation. The deviation of the Nernstian slope from the theoretical value and the term of the constant potential E° participating in the Nernstian equation should also be taken into account during the extrapolation; otherwise, the titration error will become significant. On the other hand, a small change of the initial volume of the titration solution created no serious problem on the end point. The experiment of micro-titration of HCl sample with 0.01M NaOH solution using the Gran′s plot method resulted in a reproducibility of the end point with a relative standard deviation of 0.62%, when two data points were taken at 30% and 50% of the titration fraction for the extrapolation.
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  • A Novel Amperometric Ammonia Sensor
    Toshiyuki OSAKAI, Tadaaki KAKUTANI, Mitsugi SENDA
    1987 Volume 3 Issue 6 Pages 521-526
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.521
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    A novel amperometric ammonia sensor was designed in which an amperometric ammonium-ion selective polyvinyl chloride)-nitrobenzene gel electrode containing dibenzo- 18-crown-6 was covered with a gas-permeable membrane. This sensor gave a current response proportional to the ammonia concentration in the range from 2 to 200μmol dm-3. We examined the dependence of the current response on electrode potential, thickness of the internal- solution layer, and pH of the sample solution. The results were well explained by theoretical equations.
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  • Hue Detector for Column Chromatography
    Koichi TAKAHASHI, Takakazu KATSUI, Masanori MORITA
    1987 Volume 3 Issue 6 Pages 527-530
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.527
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    A column chromatograph was made, which has an amorphous integrated diode photo-electric transducer (Sanyo, full color sensor AM 3302) as photodetector. Dyes extracted from spinach leaves were analyzed. AM 3302 has three color (red, green and blue) filters in front of the face of the photo-sensor, and transduces photo-intensities to the voltages. Three voltage outputs are taken into the microprocessor by the rapid sampling method. Three outputs, which correspond to the light intensity at three different wavelengths, form the three point spectrum. AM 3302 can be used as a simple detector of the hue. Extracted dyes from spinach leaves were separated on the silica gel column. The green and two yellow fractions were monitored by the hue detector. The green fraction was fractionated and its fast atom bombardment mass (FAB-MS) spectrum was measured and identified to be chlorophyll a by quasi molecular ion m/z 893 [M+H]+ value.
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  • Solvent Extraction-Spectrophotometric Determination of Trace Orthophosphate in Water by Stopped-Flow Time Difference Analysis Technique
    Ken-ichiro KANAYA, Keitaro HIROMI
    1987 Volume 3 Issue 6 Pages 531-534
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.531
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    For the determination of phosphate from μg l-1 to sub-μg l-1 level in water, the "stopped-flow time difference analysis" technique (a sort of end-point assay using the stopped-flow method) was used by combining the "Molybdenum Blue" method and the pre-concentrating solvent extraction of 12-molybdophosphate. Isobutyl alcohol and stannous chloride were used as the solvent and the reductant, respectively. The reducing reaction was fast and the colored complex formed by the reaction was unstable. Phosphate concentration was easily determined by analyzing the reaction curves recorded for only 0.5s. The apparent molar absorptivity of phosphate was about 2×105M-1 cm-1 at 730nm, and the detection limit was 0.3μg l-1. The calibration curve was linear from zero to 5μg l-1. The method was applied to the determination of phosphate in tap water samples; the relative standard deviation was less than 3% and the recovery of 20μg l-1 phosphate was 100±6%.
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  • Liquid-Liquid Extraction of Metal Ions by Cyclic and Acyclic Tetrathio Ethers
    Kenji CHAYAMA, Eiichi SEKIDO
    1987 Volume 3 Issue 6 Pages 535-539
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.535
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    Liquid-liquid extraction of metal ions with several cyclic and acyclic tetrathio ethers was examined using picrate as the anion of the ion pair. Three new acyclic compounds were synthesized. Class b metal such as Ag(I), Cu(I), Pd(II) and Hg(II) were extracted well, whereas class a and class ab metals were not extracted at all except for Cu(II) with each ligand, regardless of its being cyclic and acyclic tetrathio ethers. The extraction behavior of copper(I) was stoichiometrically examined. Copper(I) was extracted with five ligands(L) into 1, 2-dichloroethane as ion pair compounds, [Cu(I)L]+Pic-. The extraction constant Kex for copper(I) with each ligand was determined. Copper(I) is most effectively extracted with the tetrathio ether of the o-xylene derivative. It becomes clear that the configuration of ligands is reflected in the Kex value.
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  • Reagent Foam Test for the Detection and Semiquantitative Determination of Silver in Aqueous Solution
    A. B. FARAG, A. M. EL.-WAKIL, M. E. M. HASSOUNA, M. H. ABDEL-RAHMAN
    1987 Volume 3 Issue 6 Pages 541-542
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.541
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    The analytical suitability of dithizone foam for the detection and semiquantitative determination of traces of silver in aqueous solution has been examined. The effect of diverse ions on the detection of silver has been critically investigated. The detection limit of silver by the proposed foam batch and column methods are 0.08 ppm and 10ppb, respectively.
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  • Spectrophotometric Determination of Micro Amounts of Sulfide, Sulfite and Thiosulfate
    Tomozo KOH, Yasuyuki MIURA
    1987 Volume 3 Issue 6 Pages 543-547
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.543
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    The present method is based on the spectrophotometric measurement of an excess amount of iodine for the reaction of iodine with sulfide, sulfite and thiosulfate in a mixture after proper chemical treatments; it consists of three Procedures: I, II and III. The absorbance obtained by Procedure I corresponds to the sum of the thiosulfate and twice the sulfide and sulfite in the mixture. The absorbance obtained by Procedure II, where sulfite was masked by formaldehyde, corresponds to the sum of the thiosulfate and twice the sulfide. The absorbance obtained by Procedure III corresponds to only the amount of thiosulfate, because sulfite was masked by formaldehyde and sulfide was eliminated with the suspension of zinc carbonate hydroxide. The conditions under which all the three sulfur species in a mixture can be stable and react stoichiometrically with iodine were established. The method is applicable to the determination of sulfur species in amounts more than 0.05μmol and gave a relative standard deviation of 3% at 0.4μmol level. It has been applied to the determination of sulfide, sulfite and thiosulfate in various amounts in several fumarolic condensate samples.
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  • Fluorometric Flow Injection Analysis of Saliva for Nitrite
    Takafumi OHTA, Youichi ARAI, Shoji TAKITANI
    1987 Volume 3 Issue 6 Pages 549-551
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.549
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    A fluorometric flow injection analysis for nitrite in saliva has been developed. The fluorescent reagent, 4-hydroxycoumarin, was nitrosated with the injected nitrite in acidic medium, and reduced subsequently with sodium thiosulfate to give 3-amino-4-hydroxycoumarin, which was fluorescent in alkaline medium. Under the optimized conditions, the detection limit was 4.3×10-8M at a sample volume of 210μl, and the relative standard deviations(n=8) for 20 and 100ng/ml nitrite solutions were 2.8 and 1.7%, respectively. The sampling rate was 30 samples per hour. Saliva was diluted with water, and analyzed by the FIA system after centrifugation. The recovery data indicated that the present method was applicable to saliva samples.
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  • Simultaneous Determination of Triglycerides and β-D-Glucose by Flow Injection Analysis Using Enzyme Immobilized Open Tubular Reactors
    Shuhei YONEZAWA, Fujio MORISHITA, Tsugio KOJIMA
    1987 Volume 3 Issue 6 Pages 553-556
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.553
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    Triglycerides of clinical importance were determined by a flow injection analytical (FIA) method using whisker- walled open tubular reactors, on the inner wall of which lipoprotein lipase and glycerol dehydrogenase were immobilized. Triglycerides were measured by monitoring the resulting NADH fluorimetrically. Since all the reactions were carried out in a flowing stream, pretreatments of samples prior to analysis could be reduced to a minimum. Completion of hydrolysis of triglycerides required more than 10min, so the stopped-flow procedure was adopted at this stage. Before the peak corresponding to triglycerides appears, a glucose dehydrogenase immobilized reactor was placed as the 2nd channel in a splitting-confluence FIA system to determine another species of clinical importance, β-D-glucose; triglycerides and β-D-glucose in the concentration ranges of clinical significance could be determined simultaneously with satisfactory reproducibility.
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  • Sequence-Selective Separation of Oligonucleotides and DNA Fragments by Using Polyethyleneglycol-Bound Intercalators
    Shigeori TAKENAKA, Kunihiko DOHTSU, Naotoshi NAKASHIMA, Makoto TAKAGI
    1987 Volume 3 Issue 6 Pages 557-560
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.557
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    Anthracene; acridine and quinacrine which possess base- and sequence-selectivity in their DNA-binding (intercalating) properties were covalently bound to poly(ethyleneglycol) (PEG) via ester bonds. These PEG-bound intercalators induced the retardation of DNA restriction fragments and oligonucleotides (pentadecamers) in the electrophoresis in agarose gel and polyacrylamide gel, respectively. The pattern of mobility retardation depended on the base composition of the DNA fragments and oligonucleotides, reflecting the base selectivity of the parent intercalators. The PEG-bound intercalators also discriminated the base sequence, and the oligonucleotides of nearly sequence-isomereric structures such as (TA)7T and A8T7 were mutually readily separated.
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  • Spectrophotometric Determination of Sodium Mercaptoundecahydrododecaborate with 5, 5′-Dithiobis(2-nitrobenzoic acid)
    Isao IKEUCHI, Tameyuki AMANO
    1987 Volume 3 Issue 6 Pages 561-564
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.561
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    A simple, sensitive and accurate method for the determination of sodium mercaptoundecahydrododecaborate, Na210B12H11SH, which is one of the most useful agents for boron neutron-capture therapy of brain tumors, was developed by spectrophotometry with 5, 5′-dithiobis(2-nitrobenzoic acid) [DTNB]. The color development based on 2-nitro-5-mercaptobenzoic acid liberated from DTNB by an exchange reaction of the sulfhydryl group showed maximal absorbance at 398nm with 1.65×104dm3 mol-1 cm-1. Beer′s law was obeyed up to 6×10-4mol dm-3. The detection limit was 2×10-5mol dm-3.
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  • Determination of Aromatic Aldehydes by High Performance Liquid Chromatography after Precolumn Fluorescent Derivatization with 4, 5-Dimethyl-o-phenylenediamine
    Masatoki KATAYAMA, Yoshio MUKAI, Hirokazu TANIGUCHI
    1987 Volume 3 Issue 6 Pages 565-568
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.565
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    A new sensitive method for the determination of aromatic aldehydes (benzaldehyde, o-, m- and p-hydroxybenzaldehydes and vanillin) is described which employs high performance liquid chromatography (HPLC) with fluorometric detection. Aromatic aldehydes were derivatized with 4, 5-dimethyl-o-phenylenediamine (DMPD) in an acidic medium, and the resultant fluorescent benzimidazole derivatives were separated on a reversed phase column (Zorbax ODS) with 0.02M acetate buffer(pH 4.0)-methanol(1:1) containing 5mmol 1-1 n-dodecyltrimethylammonium bromide as a mobile phase. The detection limits of aromatic aldehydes were in the range from 0.05 to 2.5 ng ml-1. This method was applied to the determination of vanillin in commercial ice cream.
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  • Determination of 2, 3-Diphosphoglycerate in Red Blood Cells by High Performance Liquid Chromatography
    Yukihiro TAKEBAYASHI, Rumiko MITSUMA, Toshio IMANARI
    1987 Volume 3 Issue 6 Pages 569-572
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.569
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    A method for the determination of 2, 3-diphosphoglycerate(2, 3-DPG) was established by high performance liquid chromatography with spectrophotometric detection using the ferrous ion as a postcolumn labeling reagent. Chromatographic conditions were as follows: Column, Asahipak BEST 502N (5mm i.d.×100mm); eluent, 0.3M acetate buffer (pH 5.0) containig 15mM Mg(NO3)2 at a flow rate of 1ml/min; complex forming reagent, 20 mM FeSO4(NH4)2SO4 containing 1.5mM dithiothreitol and 5% sodium dodecylsulfate (0.5ml/min); detection wavelength, 260nm. The calibration curve for 2, 3-DPG was linear in the range of 1.0 to 20.0nmol, and the relative standard deviations were 2.05 and 0.79% (n=5) at 2.7 and 16.0nmol, respectively. The correlation of the present method to the conventional enzymatic method was satisfactory (r=0.999).
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  • Separation of Cobalt(II) from Nickel(II) by Using Dithizone Extraction and Rate-controlling Effect of 1, 10-Phenanthroline
    Hiroshi KAWAMOTO, Hideo AKAIWA
    1987 Volume 3 Issue 6 Pages 573-574
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.573
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  • Speciation of Arsenic Compounds in Marine Life by High Performance Liquid Chromatography Combined with Inductively Coupled Argon Plasma Atomic Emission Spectrometry
    Masatoshi MORITA, Yasuyuki SHIBATA
    1987 Volume 3 Issue 6 Pages 575-577
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.575
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  • A New Polymeric Pentafluorobenzylating Reagent for Gas Chromatography
    Yuta YASAKA, Toshio NAGASAKA, Minoru TANAKA, Koichi FUNAZO, Hsin-Lung ...
    1987 Volume 3 Issue 6 Pages 579-580
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.579
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  • Flow Injection-Fluorometric Determination of Amino Acids Utilizing Enhanced Catalytic Reaction
    Hisakazu MORI, Kazue NATSUME
    1987 Volume 3 Issue 6 Pages 581-582
    Published: 1987
    Released on J-STAGE: July 27, 2007
    DOIhttps://doi.org/10.2116/analsci.3.581
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  • Porous Membrane Phase Separator in Solvent Extraction
    Kousaburo OHASHI, Syozo KOKUBO, Shohei TAMURA, Katsumi YAMAMOTO
    1987 Volume 3 Issue 6 Pages 583-584
    Published: December 10, 1987
    Released on J-STAGE: June 27, 2006
    DOIhttps://doi.org/10.2116/analsci.3.583
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