BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 51, Issue 5
Displaying 1-9 of 9 articles from this issue
Research Papers
  • Nobuo NAKANO, Yasuhiro TERAUCHI, Tetsuya KAWABE, Kunio NAGASHIMA
    2002 Volume 51 Issue 5 Pages 293-298
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    A porous cellulose tape impregnated with a processing solution that includes sodium nitroprusside dihydrate, zinc formate, glycerin and methanol is a highly sensitive means of detecting sulfur dioxide in air. When the sample including sulfur dioxide was passed through the tape, sulfur dioxide was absorbed on the surface of the tape, and reacted with zinc nitroprusside to form a stain. The intensity of the stain was proportional to the concentration of sulfur dioxide at a constant sampling time and flow rate, and it could be recorded by measuring the intensity of reflecting light (555 nm). The detection limit was 0.03 ppm for sulfur dioxide with a sampling time of 20 s and a flow rate of 400 ml/min. Reproducibility tests showed that the relative standard deviation of response (n = 8) was 0.97% for 2 ppm sulfur dioxide (TLV-TWA for sulfur dioxide is 2 ppm). No interference was observed from acetylene (0.5%), ethanol (1 vol.%), acetone (1 vol.%), trichloroethylene (1 vol.%), carbon dioxide (99.9 vol.%), carbon monoxide (103 ppm), hydrogen chloride gas (5 ppm), ammonia (40 ppm), nitrogen dioxide (50 ppm), hydrogen sulfide (20 ppm).
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  • Hideo HAYASHI, Tomokazu TANAKA, Masataka HIRAIDE
    2002 Volume 51 Issue 5 Pages 299-303
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    Although ICP-MS offers a powerful multielement analytical method, the mass spectral interference due to argon often becomes a serious problem. For example, 40Ar16O+, 40Ar35Cl+ and 40Ar2+ interfere with the determination of 56Fe+, 75As+ and 80Se+, respectively. Therefore, we replaced argon by helium to develop an interference-free ICP-MS, and successfully detected iron and arsenic in aqueous solutions. Some weak background peaks, however, were still generated at m/z 79∼82 and disturbed the determination of traces of bromine (79Br+) and selenium (80Se+). In the present work, it was found that these peaks originated from the copper interface by a secondary discharge. They were assigned to 63Cu16O+, 63Cu16OH+, 65Cu16O+ and 65Cu16OH+. The nickel interface caused more serious background at m/z 50∼100. On the other hand, no spectral interference was observed over a wide m/z range when the interface was constructed from aluminum. The optimized helium ICP-MS was used for the determination of traces of bromine and selenium in water. A 5 μl volume of a sample was placed and heated electrothermally on a tungsten filament. The resulting vapor was introduced into the helium plasma for a mass spectrometric analysis. The relative standard deviation of the signals (10 ng ml-1, n=10) was approximately 10%. The detection limits based on 3σ were 0.2 ng ml-1 for Br and 0.09 ng ml-1 for Se, which were lower compared with the conventional argon ICP-MS (Br 20 ng ml-1, Se 0.25 ng ml-1).
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Technical Papers
  • Norio MANABE, Hiroaki MINAMI, Yoshimitu YOKOTA, Fumiaki OKUDA, Yuuya U ...
    2002 Volume 51 Issue 5 Pages 305-310
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    After a pretreatment of methanol added thermal decom-position, GC was applied to the simultaneous determi-nation of a popular amino triazole-type copper deactivator, 3-(N-salicyloyl) amino-1,2,4-triazole (CDA-1, abbreviation: CDA) and a hindered phenol-type antioxidant, tetrakis[methylene 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]methan (Irganox1010, abbreviation: IRG). Their contents for several polypropylene standard samples, prepaired by adding 0.2 to 1.0 wt% of each CDA and IRG, were determined based on the peak intensity of the components decomposed with methanol at 220°C for 1.5 h in a sealed pyrex tube. The relative standard deviations (RSD) were 3.1 to 5.9%. This technique can be used to determine the CDA andIRG contents simultaneouly and to evaluate the degradation process of polymer materials.
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  • Takeshi YAMANE, Takashi MURAYAMA, Toshihisa MARUTA, Takaji KAWAI
    2002 Volume 51 Issue 5 Pages 311-315
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    A flow-injection system (FIA) is described for the simple and rapid determination of chromium(VI) in a leached solution from soil, which allows to one simultaneously measure the signal responses due to chromium(VI) and a blank. The method utilizes a color-forming reaction of CrVI with diphenylcarbazide (DPC). The system is based on the synchronized injection of a large volume of sample solution and a small volume of a modifying reagent solution (ascorbic acid for reducing CrVI to CrIII) into separate streams, which are then merged at a confluence point. Thus, two reaction zones, for CrVI and for the blank, in a single sample plug are provided, and then mixed down stream with a stream of DPC for spectrophotometric detection. The variables related to such a reaction and which provide two reaction zones were studied in detail, and optimal conditions and manifold were established. The calibration graph was rectilinear in the range of 0.005∼0.2 mg/l CrVI. A relative standard deviation (n=5) of 1.1% was obtained for the analysis of 0.05 mg/l CrVI solution. The estimated limit of determination was 0.005 mg/l. An analysis rate of 10/h is estimated. The results for analysis of various solutions leached from soil by the proposed FIA system correspond well with those by the standard batchwise method. The proposed FIA system can afford a rapid and simple analysis: only 6 min is required for analytical measurement after sample injection, and no complicated manual operation is involved.
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Technical Letters
Digest of Doctoral Dissertation
  • Hideki KURAMITZ
    2002 Volume 51 Issue 5 Pages 327-328
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    Some simple methods for an electrochemical binding assay for protein-ligand like avidin-biotin and lectin-sugar were developed. In a homogeneous binding assay based on the use of an electroactive label, following methods are proposed to obtain a sensitive electrochemical response. 1) In order to obtain an amplified electrode response without an enzyme label, an electron-transfer mediator was used as a label. 2) In order to use anodic stripping voltammetry for the sensitive detection of metal, a ligand labeled with a complex reagent was applied to the binding assay. 3) An accumulation of ligand to an ion exchange membrane electrode was investigated using a ligand labeled with a cationic electroactive molecule. 4) A highly sensitive detection of an electroactive labeled ligand was attempted by the potential regulating accumulation on a plain glassy carbon electrode. In a heterogeneous binding assay based on a technique without a label, some hydrophilic electroactive compounds were used as a redox marker to evaluate the protein-ligand interaction. A sensitive and selective binding assay could be achieved by monitoring the change in the electrode response of the redox marker. In addition, a development of screening method for endocrine disrupting chemicals using 17β-estradiol labeled with an electroactive compound was attempted. These electrochemical binding assays do not require a separation procedure prior to any measurements. Therefore, dynamic monitoring for the formation of the protein-ligand complex is possible.
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  • Hong-Bing HOU
    2002 Volume 51 Issue 5 Pages 329-330
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    Simple methods for the chemical speciation of antimony and organotin compounds were developed by atomic spectroscopy. Antimony was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and high-resolution inductively coupled plasma mass spectrometry (ICP-MS) with a hydride generation technique. Stibine generated with sodium tetrahydroborate(III) (SBH) in a mixing coil was separated from solution with a spiral tube in a closed vessel. The antimony contents of River Arakawa were determined by the present methods. Antimony(III) and antimony(V) were determined differentially by ICP-AES and ICP-MS. Antimony(III) was determined at pH 5.5, while the total antimony was determined at pH 1.0 using potassium iodide as a prereductant. It was found by ICP-MS that the antimony(III) contents of River Arakawa increased while the antimony(V) contents decreased while descending down-stream. Tributyltin and triphenyltin in fish were determined by gas chromatography-atomic absorption spectrometry (GC-AAS) with hydride generation. Fish meat was homogenized in a hydrochloric acid solution of 8-quinolinol. The chlorides in fish were extracted into hexane. After the solvent had been converted to 2-propanol, the solution was applied to a Bondesil SCX solid sorbent. The organotin compounds were eluted with a methanol solution of hydrochloric acid and determined by GC-AAS after hydradization with SBH. The organotin chlorides are supposed to form ion-associates with 8-hydroquinolinium cation in a hydrochlic acid medium.
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  • Yong-Lai FENG
    2002 Volume 51 Issue 5 Pages 331-332
    Published: May 05, 2002
    Released on J-STAGE: March 13, 2009
    JOURNAL FREE ACCESS
    Tin was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and high resolution-inductively coupled plasma mass spectrometry (ICP-MS) with a hydride generation technique. Stannane generated with sodium tetrahydroborate(III) (SBH) was separated from solution with a spiral tube in a closed vessel. The tin content in marine materials was determined by the present methods. Antimony(III) and antimony(V) were determined by ICP-AES or ICP-MS using the pre-reduction of antimony with L-cysteine. Also, arsenic(III) and arsenic(V) were determined by ICP-MS combined with the pre-reduction of arsenic. Tributyltin and triphenyltin in marine sediments were determined by gas chromatography-atomic absorption spectrometry (GC-AAS) with hydride generation. The chlorides in sediments spiked with a hydrochloric acid solution of 8-quinolinol were extracted into toluene. After the solvent had been converted to ethanol, it was applied to a Bondesil SCX. The organotin compounds were eluted with a methanol solution of hydrochloric acid and determined by GC-AAS after hydridization.
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