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ONLINE ISSN: 1883-2954
PRINT ISSN: 0021-1575

Tetsu-to-Hagané Vol. 89 (2003), No. 9

  • Determination of Some Trace Elements in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique

    Akihiro MATSUMOTO, Taketoshi NAKAHARA

    pp. 881-889

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    Abstract

    A high power microwave induced plasma (MIP) source using an Okamoto cavity can be sustained by He, N2 and air at atmospheric pressure. The cavity has been originally developed to produce an alternative analytical ionization source to argon inductively coupled plasma (ICP) for mass spectrometry (MS). This review introduces that an annular-shaped high power (1.0 kW) nitrogen microwave induced plasma (N2-MIP) sustained at atmospheric pressure by Okamoto cavity, as a new excitation source for atomic emission spectrometry (AES), has been demonstrated. Subsequently the combination of high power N2-MIP-AES with the continuous-flow hydride generation method was examined for the determination of such hydride-forming elements as arsenic, selenium, antimony, tellurium and bismuth. Moreover, the same technique has been extended for two (arsenic and antimony)- and three-element (arsenic, antimony and bismuth) simultaneous determination. After the interference study, the present method has been applied to the determination of trace concentrations of the above-mentioned hydride-forming elements in several steels reference materials. The results obtained by this method were in good agreement with their certified values.

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    1. Determination of Bismuth in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique Tetsu-to-Hagané Vol.89(2003), No.9
    2. Simultaneous Determination of Arsenic and Antimony in Steels and Pure Coppers by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique Tetsu-to-Hagané Vol.88(2002), No.5
    3. Simultaneous Determination of Arsenic, Bismuth and Antimony in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Method Tetsu-to-Hagané Vol.89(2003), No.5

  • Comparison of ICP Atomic Emission Intensities on Axial and Radial Views, and Determination of Trace Amounts of As, Sb and Sn in Iron and Steel

    Toshiko ITAGAKI, Kunio TAKADA, Kazuaki WAGATSUMA, Kenji ABIKO

    pp. 890-894

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    Abstract

    Trace amounts of As, Sb and Sn in iron and steel were determined by ICP-OES. Intensities of some atomic emission lines were simultaneously determined from axial or radial view of argon plasma. Atomic emission intensities from the axial view were higher about 37 to 53 times than those from the radial view. Detection limits of As, Sb and Sn were order of 1 ppm in iron and steel by axial view measurement. Detection limit of As was lowered to order of 0.1 ppm after removal of iron as main component in sample solution with co-precipitation of MnO2.

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    1. Rapid Evaluation of Inclusion in Steel by Use of Cold Crucible Levitation Melting Tetsu-to-Hagané Vol.89(2003), No.9
    2. Simultaneous Determination of Arsenic and Antimony in Steels and Pure Coppers by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique Tetsu-to-Hagané Vol.88(2002), No.5
    3. Simultaneous Determination of Arsenic, Bismuth and Antimony in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Method Tetsu-to-Hagané Vol.89(2003), No.5

  • Analysis of the Trace Amount of Metallic Elements in Iron and Steels Using the Microwave Decomposition by ICP-AES and ICP-MS

    Kazutoshi HANADA, Yoshihisa KAJIMA, Kyoko FUJIMOTO, Makoto SHIMURA, Susumu SATOH

    pp. 895-899

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    Abstract

    Trace amount of metallic elements as Al, Ca and Mn, which form oxides in iron and steels, were determined by ICP-AES and ICP-MS after the decomposition of samples using HF/HCl/HNO3 under microwave irradiation. The oxides in iron and steels, which were extracted by using Br2-CH3OH extraction, could be decomposed by two-steps acid decomposition using H2SO4 followed by addition of HF in a pressurized vessel at elevated temperatures. The limits of detection for Al, Ca, Mg, Mn, Cr, Ni, Cu, Zn and Co by microwave decomposition/ICP-MS were 0.010.36 ppm.

  • Determination of Trace Tramp Elements and Other Trace Elements in Pure Iron Standard Materials by Instrumental Neutron Activation Analysis

    Yukiko OKADA, Shoji HIRAI

    pp. 900-905

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    Abstract

    Trace tramp elements (Zn, As, Sn and Sb) and other trace elements in pure iron certified standard materials, JSS003-4, JSS168-7 and JSS172-7, prepared by the Iron and Steel Institute of Japan were determined by instrumental neutron activation analysis (INAA). Four aliquot samples of each certified standard material (ca. 100-450 mg) were irradiated for 6 h at a thermal neutron flux of 3.7 × 1012 n cm-2 s-1 in the Rikkyo University Research Reactor. The irradiated samples were measured by γ-ray spectrometry using a coaxial Ge detector. The concentration of 3 elements (Co, Ni and As) in the JSS003-4, the concentration of 7 elements (Cr, Co, Ni, As, Mo, Sn and Sb) in JSS168-7 and the concentration of 7 elements (Cr, Co, Ni, As, Mo, Sb and Ta) in JSS172-7 were determined. The determined values were in good or nearly good agreement with the certified values or the reported values. The lower limit of determination values for the tramp elements were 0.01-0.1, μg/g Sb and As and 10-100 μg/g Zn and Sn respectively.

  • Simultaneous Determination of Trace Copper, Lead, Cadmium and Zinc in Iron and Steel by Stripping Analysis

    Tatsuhiko TANAKA, Tomohiro KASHIHARA, Atsushi TAGUCHI, Hiroyuki KONDO

    pp. 906-913

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    Abstract

    A simple and reliable method is described for the simultaneous determination of copper, lead, cadmium and zinc at the μgg-1 level in iron and steel by two different stripping techniques without any preliminary separation of the iron matrix. Constant current stripping analysis (CCSA) at a mercury-coated glassy carbon electrode was compared with anodic stripping voltammetry (ASV) at a hanging mercury drop electrode. Analyte ions in nitric-sulfuric acid mixture solutions (pH=4 for ASV) were electrodeposited on the working electrode with stirring at a controlled potential for 3 to 10 min. The deposits were then anodically stripped at a constant current of +30μA for CCSA or in the potential range -1.2 to -0.2V vs. SCE at a scan rate of 20mVs-1 by a differential pulse mode for ASV. The interference of iron(III) was eliminated by reducing it with L(+)-ascorbic acid to iron(II). The influence of foreign elements on the determination was evaluated. The lower limits of determination for CCSA and ASV were 50 and 0.5μgg-1 of lead, cadmium and zinc in iron and steel, respectively. Differential pulse ASV had high sensitivity and poor peak resolution compared with CCSA. The simultaneous determination of 5 to 60ugg-1 of these four elements in iron was achieved with the relative standard deviations (n=5) of less than 7% within 12 min. Recoveries for the analytes ranged from 88 to 108%. The proposed methods can be also applied to the simultaneous determination of tramp elements in obsolete steel scrap.

  • Determination of Zinc in Iron and Steel by Reversed-phase High-performance Liquid Chromatography with α, β, γ, δ-tetrakis(4-carboxyphenyl)porphine as a Precolumn Derivatizing Agent

    Nobuo UEHARA, Kazutomo NOMOTO, Tokuo SHIMIZU

    pp. 914-919

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    Abstract

    A novel method for the determination of trace amounts of zinc in iron and steel has been demonstrated by a reversed-phase HPLC using α, β, γ, δ-tetrakis(4-carboxyphenyl)porphine as a derivatizing reagent. Certified reference materials of iron and steel were used to prepare digestive samples by decomposition followed by 4-methyl-2-pentanone extraction and sulfuric acid fuming. The digested sample solutions were derivatized with Cd(II)-α, β, γ, δ-tetrakis(4-carboxyphenyl)porphine solution in ammonium buffer (pH 9.0) solution, using 5-sulfosalicylate as a masking reagent. Aqueous-acetonitrile (45:55 w/w) containing 7.0 × 10-2 mol kg-1 of lactate buffer (pH 4.15) was used as an eluent and was monitored at 422 nm.
    A linear calibration was observed in the concentration range from 1 × 10-8 mol dm-3 to 1 × 10-6 mol dm-3. The detection limit (3σ) of Zn(II) was 1.3 × 10-9 mol dm-3, which corresponded to 0.32 ppm in iron and steel samples. The recoveries of zinc added to the digested solution of iron and steel were with in 97 to 107%. The good recovery and high sensitivity indicate that the proposed system is of great promise for the determination of zinc present in iron and steel.

  • Spectrophotometric Determination of Antimony in Steels by Flow Injection Analysis Using a Teflon Tube Concentration Method

    Kunihiro WATANABE, Takashi OSAWA, Masayuki ITAGAKI

    pp. 920-926

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    Abstract

    Flow injection analysis of antimony in steels using a Teflon (PTFE) tube concentration method was investigated. Antimony reacted with chloride ions in hydrochloric acid solution to form a complex ion SbCl6-. The hexachloroantimony complex anion was adsorbed on the Teflon tube inner surface as ion pair, which was formed with Co(III) complex of 2-(5-chloro-2-pyridilylazo)-5-diethylaminophenol (Co-5-Cl-PADAP). The concentrated ion pair was eluted with 99% methanol, and then the absorbance of the eluate was measured at 560 nm. Excess reagent was adsorbed on the Teflon tube the same as the ion pair, so that reagent blank values were increased with excess reagent. Therefore, the conditions for the removal of excess reagent were examined. As a result, an 8% methanol solution was selected as a rinsing solution, and the removal was carried out for 3 min. The apparatus used in this flow system has four channels. One of them was a 99% methanol eluent. Others were a sample solution containing antimony, hydrochloric acid and sodium nitrite at 1.5 mllmin, a 3×10-5M Co-5-Cl-PADPAP solution at 0.2 m/lmin, and an 8% methanol at 1.3 mllmin. The calibration curve was constructed under optimum conditions by the proposed flow system. A linear relationship between the absorbance and antimony concentration was obtained over the range 0 to 50 ppb. The limits of detection and determination for antimony were 0.3 and 0.9 ppb, respectively. The determination results for antimony in steel certified reference materials showed good agreements with the certified values. The relative standard deviation for 20 ppb Sb was 0.9% (n= 6). The iron as matrix did not interfere with the determination of Sb up to a million-fold to antimony amount.

  • Determination of Arsenic in Steel by Metal Furnace-AAS and Flow Injection Analysis Based on Method with On-line Iodide Trace Extraction System

    Akio SAKURAGAWA, Tetsuyuki TANIAI, Atsushi UZAWA

    pp. 927-934

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    Abstract

    An automated on-line solvent extraction system has been developed for the determination of arsenic in steels by electrothermal atomic absorption spectrometry (ET-AAS) or flow injection analysis (FIA) based on the molybdenum blue reaction. It is based on the reaction of As(III) with iodide ion in the concentrated hydrochloric acid medium to produce AsI3, which is extracted into benzene and back-extracted into water. Because of an easy separation of water phase and benzene phase, a gravitational phase separator column was used in the automated on-line solvent extraction system. It was not utilized a membrane type phase separator so that the proposed automated on-line solvent extraction system was obtained with long-term stability, low solvent consumption and high reproducibility. Using the proposed automated on-line solvent extraction system, arsenic contained in the acid decomposed steel sample solution was automatically extracted into the benzene phase and it was back-extracted into the water phase. Then, the back-extracted water phase was used for the determination of arsenic by ET-AAS or FIA. When the ET-AAS method used for the determination of arsenic, 800 mg dm-3 of cobalt solution had to use as the matrix modifier to remove an effect of coexisted substances such as iodide ion. In this method, a determination limit of As is 0.2μg in the 0.1g of steel sample. When the FIA method used for the determination of arsenic, a determination limit of As was 1.0μg in the 0.1g of steel sample.

  • Determination of Zinc in Steel Samples by Atomic Absorption Spectrometry Using Flow System Removing Iron(III)

    Hitoshi ASANO, Hideyuki ITABASHI, Hiroshi KAWAMOTO

    pp. 935-938

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    Abstract

    An extractive-flow system, to remove iron(III) from a steel sample solution, was developed. In the flow system, the iron(III) was precipitated as hydroxide and then quantitatively extracted into the organic phase containing di(2-ethylhexyl)phosphate as extractant. The system was applied to atomic absorption spectrometry (AAS) of zinc in a standard steel sample. The result, in which the zinc concentration obtained was consistent with the certified one, showed feasibility of the proposed method as pretreatment system for the AAS of zinc in a steel sample.

  • Sensitive Determination of Molybdenum in Steel by Flow Injection-On-line Ion-exchange Preconcentration-ICP-Atomic Emission Spectrometry

    Tatsuya SEKI, Koichi OGUMA, Yoichi ISHIBASHI

    pp. 939-942

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    Abstract

    A sensitive method for the determination of molybdenum in steel has been developed by flow injection-online ion-exchange preconcentration-ICP-AES. Sample is decomposed with a mixed acid by a microwave-assisted digestion. Excess acids are removed by evaporation and the residue is taken up in 0.05 M sulfuric acid and an 50μl aliquot of the sample solution is injected into the flow injection analysis system. Molybdenum in the sample solution is adsorbed on a TEVA resin column and then eluted with 7 M nitric acid. The effluent containing molybdenum is introduced directly into a ultrasonic nebulizer of ICP-AES. The valves and pumps in the flow system are operated automatically by a personal computer. The analytical results obtained for molybdenum at a 0.01 m/m% level in the steel certified reference materials are in good agreement with certified values and the precision (R.S.D.=2.3-2.5%) is satisfactory. The detection limit estimated as 3σ of the background noise is 0.8 ng molybdenum, which corresponds to 8 μg Mo/g when 50 mg of steel sample is analyzed.

  • A Novel FI System for Chemical Analysis of Stainless Steels for Nickel Determination without Complicated Procedures and a Great Deal of Skill

    Takeshi YAMANE, Yumi TSUCHIYA, Yasuhiro TANAKA, Kyoko FUJIMOTO

    pp. 943-947

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    Abstract

    A novel flow injection (FI) system is presented for the determination of nickel as one of major constituents in stainless steel. The in-line cation-exchange separation of nickel from matrix iron and chromium utilising tartrate solution as an eluent is directly coupled with photometric detection in a continuous flow system. The photometric detection system developed here exploits the formation of water soluble complex of nickel with dimethylglyoxime in the presence of iodine as oxidizing agent in a NaOH basic media. The FI manifold and the optimum reaction conditions were established in order to achieve the simple and precise determination of nickel. A sample solution prepared by dissolving steel sample in aqua regia and diluting to the volume with water can be directly injected into the flow injection system and thus no labonus complicated manual operations for pretreatment of sample solution is needed. The present FI system offers many advantages, especially with respect to simplicity and rapidity, permitting the precise determination of nickel in a wide range of contents % with a short analysis time (<15 min) and a precision less than 1% and without a great deal of skill. The analytical results by the proposed FIA system for four Japanese Iron and Steel Certified Reference Materials (JSS CRMs) agreed well with the cerified values for nickel.

  • Flow Chemiluminescent Determination of Chromium in Stainless Steel

    Kenji MUTO, Kenichi OHNO, Jin-Ming LIN, Masaaki YAMADA

    pp. 948-952

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    Abstract

    A simple and rapid flow injection (FI) chemiluminescence (CL) method is described for the skill free-determination of chromium in stainless steel. The method is based on the measurement of light emitted from the CL system, Brilliant sulfoflavine (BSF)-H2O2-NaOH-CH3CN. The CL is considered to be BSF-sensitized emission, which results from the energy transfer to BSF from singlet oxygen molecules produced through the decomposition of H2O2 by Cr3+. Interferences from Fe3+ and Ni2+ are reduced by the addition of citrate. The analytical results for stainless steel samples by the proposed method agreed well with the certified values for chromium. The advantages of the proposed method are that Cr3+ can be determined with a short analysis time (30 samples/h), good repeatability (ca. 1% R.S.D. in stainless steel analysis) and without any special pretreatment.

  • Determination of Bismuth in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique

    Akihiro MATSUMOTO, Tadashi SHIOZAKI, Taketoshi NAKAHARA

    pp. 953-957

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    Abstract

    Trace amount of bismuth was determined by an annular-shaped high power (1.0 kW) nitrogen microwave induced plasma (N2-MIP) atomic emission spectrometry (AES) with hydride generation technique. Under the optimized experimental conditions, bismuth was determined at Bi I 223.061 nm line by use of N2-MIP-AES coupled with hydride generation, and the best attainable detection limit was 102ng/ml with a linear dynamic range of 30 to 30, 000ng/ml. The presence of several diverse elements and ions was found to cause more or less depressing interferences with the proposed technique. This method was applied to the determination of trace amounts of bismuth in steels. When bismuth in steels was determined, a large amount of Fe(III) in the solution caused a severe depressing interference, while the presence of Fe(II) showed little or no significant interference. Of the several interference-releasing agents examined, thiourea was found to be the most preferable to reduce Fe(III) to Fe(II). The present method has been applied to the determination of bismuth in steels. The results obtained by the proposed method agreed satisfactorily with the certified values.

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    2. Simultaneous Determination of Arsenic and Antimony in Steels and Pure Coppers by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Technique Tetsu-to-Hagané Vol.88(2002), No.5
    3. Simultaneous Determination of Arsenic, Bismuth and Antimony in Steels by High Power Nitrogen Microwave Induced Plasma Atomic Emission Spectrometry Coupled with Hydride Generation Method Tetsu-to-Hagané Vol.89(2003), No.5

  • Determination of Trace Elements in High Purity Iron by Solid Phase Extraction Using Bonded Silica/ICP-MS

    Shin-ichi HASEGAWA, Kunikazu IDE, Takeshi KOBAYASHI, Koichi SATO, Shukuro IGARASHI, Kunishige NAITO

    pp. 958-961

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    Abstract

    We attempted a simple pretreating method consisting of solid phase extraction using bonded silica with benzenesulfonic acid (SCX) as the solid phase sorbent to determine trace elements in pure iron samples by means of inductively coupled plasma mass spectrometry (ICP-MS). The isotope dilution method was used along with the method mentioned above to ensure precise determination of Zn. We dissolved the sample of 1.00 g by nitric acid, subsequently adding citric acid as masking agent. The analytes could be separated by 1-10 phenanthroline as chelate from the matrix by solid phase extraction after adjusting the pH and adding 1-10 phenanthroline. The optimum condition for iron separation was 0.01 kmol. m-3 1-10 phenanthroline, 10 cm3; citric acid (10 w/v%), 10 cm3; pH, 5.5; SCX, 0.5 g as the solid phase sorbent; and nitric acid, 2 cm3 as eluate. In this method, some trace elements such as Ni, Cu, Cd and Zn were determined by ICP-MS using the eluate. The limits of detection in ng/g were Ni 0.29, Cu 0.10, Cd 0.20 and Zn 0.15. We precisely determined the Zn content by jointly using the isotope dilution method.

  • Determination of Tramp Elements in Iron and Steel by Glow Discharge Mass Spectrometry

    Shinji ITOH, Hitoshi YAMAGUCHI, Isao HAMANO, Toshiyuki HOBO, Takeshi KOBAYASHI

    pp. 962-966

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    Abstract

    We examined the capability of Glow Discharge Mass Spectrometry to quantitatively analyze iron and steel for tramp elements at 10 mass ppm or less. We used 28 JSS and NIST standard reference materials to experimentally obtain the RSF (relative sensitivity factor) values for Cu, Zn, As, Sn, Sb, Pb and Bi. Systematic difference between two groups of the samples was found in the RSF values of Sb. Variation of the RSF values was large in Sn, as resulted in RSD being 7.67%, whereas Zn and Bi gave favorable results with RSD within 2%. We confirmed that the GDMS could satisfy the desired 10% accuracy for analyzing iron and steel for most of the tramp elements.

  • Evaluation of Chemical Compositions as to Pure Iron and Pure Aluminum

    Yoichi ISHIBASHI, Shoji HIRAI, Kazutoshi KAKITA

    pp. 967-972

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    Abstract

    Evaluation of trace elements in a pure iron and a pure aluminum was performed. The definitive analysis methods of steels and aluminums such as gravity, titrimetry and coulometry are applicable only for high concentration range of elements. In order to develop the definitive methods for low concentration ranges, a study group with national laboratories and steel maker laboratories was organized. The round robin tests showed that the found value by ID-ICP-MS (Isotope Dilution Inductively Coupled Plasma Mass Spectrometry) have good accuracy and good coincidence with the certified values. The found values by ICP-MS have good coincidence with certified values and/or with the found values by NAA (Neutron Activation Analysis). Trace elements less than 1 ppm could be determined by ICP-MS, however the precision should be improved by standardizing the method. The found values by both ID-ICP-MS and ICP-MS have good repeatability. Oxygen in pure iron was evaluated by round robin test using the inert gas fusion method and CPAA (Charged Particle Activation Analysis) method. Evaluation of surface-oxygen at pure iron was investigated.

  • Spectrophotometry of Boron in Steels with Curcumin by Flow Injection Analysis

    Kunihiro WATANABE, Atsushi SHISHIDO, Masayuki ITAGAKI

    pp. 973-978

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    Abstract

    The determination of boron in steels was investigated by flow injection analysis (FIA) using curcumin, which has been used for the conventional spectrophotometry of boron. The conventional curcumin method requires the evaporation of the sample solution to dryness in the procedure. Therefore, the curcumin method has been not adapted for FIA. The use of acetic anhydride could alternate the evaporation process in the conventional method. This enables us to apply curcumin to FIA to remove the coordinated aqueous molecule from boron. The flow system was composed with five channels including the concentration column (Amberlite IRA743). The 2 × 10-3M curcumin (acetic acid: acetic anhydride=1 : 4 v/v), the mixed acid (sulfuric acid: acetic acid: acetic anhydride =1 : 6 : 13) and 0.1 M sodium hydroxide were used to form boron curcumin complex as the reagent solutions. By using the concentration column, boron was separated from matrix iron (10000 ppm), and was concentrated to 13-fold in 0.42 ml of 10% sulfuric acid as eluent. The obtained calibration curve was linear over the range of 0-100 ppb in the sample solution. The limit of determination (10 Sb) was 2 ppb in the sample solution. The analytical results for boron in standard steel samples (B: 0.001-0.0106%) show good agreement with the certified values.

  • Characteristics of Liquid Core Waveguide Cell Made of Low-refractive-index Polymer and Its Application to the Spectrophotometric Determination of Sulfur in a Steel Sample

    Kin-ichi TSUNODA, Tomonari UMEMURA, Takashi WATANABE, Hiromi TAKIGUCHI, Hitoshi ASANO, Hideyuki ITABASHI, Yohichi ISHIBASHI, Sakae SATO

    pp. 979-981

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    Abstract

    Teflon AF-2400 capillary (i.d. 0.29 mm, o.d. 0.5 mm) was used as a liquid core waveguide cell with an aqueous solution sample. The refractive index of the Teflon AF-2400 capillary (n=1.29 (632.8nm)) is lower than that of water (nD=1.33), thus, the capillary formed a liquid core waveguide and was elongated up to 117 cm long. The sensitivity in detecting methylene blue with the 30 cm capillary cell was enhanced about 32-fold in comparison with that of a conventional cell (1cm). The cell (30cm) was applied to the spectrophotometric determination of sulfur in a standard steel sample after distillation of sulfur as hydrogen sulfide.

  • New Device of High Sensitive and Simplified Detection System for Sulfur by Means of Mist-Gas Phase Chemiluminescent Reaction Associated with Skill-free Technology in Steel Analysis

    Naoki OMI, Mikita ISHII, Yumi KATO, Masaaki YAMADA

    pp. 982-987

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    Abstract

    In relation to a skill-free technology in steel analysis, a new mist-gas phase chemiluminescent detection system for sulfur was devised to be coupled with a flow injection technique. The proposed system was composed of two manifolds of 8.0×10-4M KMnO4 and 1.0×10-4M riboflavine phophate at pH 2.5 adjusted with H2SO4 and H2S in N2 balance and a chemiluminescent detection system. The reaction cell was made by a spherical glass flask of about 100 mm i.d.. An outlet of the spherical glass was connected with the nebulizer system, which was constructed by the triplicate tubing system of 0.5 mm i.d. brass, 5 mm i.d. pyrex glass having 0.8 mm i.d. at the edge and 4.5 cm i.d. vinyl chloride at the inside in order. The analysis was performed by a 5 sec injection of the chemiluminescent reagents at 10 ml/min into the continuous H2S sample flow at 7.5 l/min. Sulfur content was indirectly determined in terms of that of H2S. The chemiluminescent reaction scheme of H2S was supposed to be same as in that of SO2. In the optimized operating condition, the lower detection limit was 0.5 ppm and a calibration for the determination was linear between 0.5 ppm and 3.0 ppm. A reproducibility of the determination was less than 1% in terms of RSD at more than 10 repeating runs in 0.5 ppm, 1.0 ppm and 2.0 ppm H2S concentrations. Analytical time required was less than 10 s for one sample. Their analytical figure of merits were usable for the skill-free grade technique in future.

  • Development of Determination of Trace Oxygen in Steel Using Molten Tin after Removing Surface Oxide under the Closed System

    Hiroshi UCHIHARA, Atsushi BANDO, Masahiko IKEDA, Taketoshi NAKAHARA

    pp. 988-993

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    Abstract

    The trace oxygen analysis in steel is usually measured by infrared method after fusion under inert gas. For the high accuracy analysis of the trace oxygen, it is necessary to remove completely the oxide of the sample surface ahead of the determination. Also it is important to decrease the carbon monoxide gas evolved from the graphite crucible. The sample after the surface oxide is removed is oxidized easily or adsorbs moisture. Therefore, it is necessary to analyze without exposing the sample to atmosphere after the oxide film is removed. Then, to take out the sample in the graphite crucible in the closed system, the mechanism of impulse furnace has been improved. To remove the oxide film of the sample surface, the sample was heated for 60 sec by the inert gas fused furnace of 1000°C. The sample was cooled down to the room temperature in the impulse furnace. The sample was taken out of the graphite crucible with a magnet stick after granule Sn was dropped in the closed system. The sample and the magnet were kept above the upper electrode in the closed system. Afterwards, oxygen in Sn was reduced to carbon monoxide gas and removed by heating at 2400°C of the temperature in which the sample was analyzed. When the base line became a constant, the output signal was initialized. The sample kept with the magnet was dropped and melted. Oxygen was reduced to the carbon monoxide, and measured with the non-dispersion infrared detector. The analytical result of the oxygen of steel sample JSS GS-6b (oxygen concentration 3.4 μg·g-1) that removed the surface oxygen was 2.9μg·g-1, and the standard deviation was 0.05 μg·g-1. This standard deviation has been improved to past 1/4.

  • Development of Continuous Monitoring System for Gas Generation Behavior during Coking Reaction

    Masayuki NISHIFUJI, Yuji FUJIOKA, Koji SAITO

    pp. 994-999

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    Abstract

    For characterizing coking reaction, it can be important information to realize gas generation behavior on pyrolysis of coal. In this study, a new monitoring system for gas generation behavior during coking reaction has been established. This system consists of main three parts, carrier gas supplier part, reaction part with a tube in an electric furnace and detector part of Fourier-transform infrared spectroscopic analyzer (FT-IR) and of a sensor for hydrogen. Coal sample in nitrogen flow was heated with an electric furnace, and generated gas was lead to FT-IR and a gas sensor with nitrogen gas carrier. This method has a good time-resolved of second order, so that a short time reaction of coal pyrolysis can be monitored continuously. Using this system, different gas profiles on coking reaction of two coals with opposite characters could be obtained. This system is great effective in detailed characterization of coal pyrolysis, because it is able to monitor continuously the reaction with in-situ to high temperature (more than 600°C) it cannot be examined by any other methods.

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  • Rapid Evaluation of Inclusion in Steel by Use of Cold Crucible Levitation Melting

    Hiroyuki KONDO, Takehiko TOH, Ryuji UEMORI, Tokio SUZUKI, Koichi CHIBA, Hideaki YAMAMURA, Masamitsu WAKOH, Eiichi TAKEUCHI

    pp. 1000-1004

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    Abstract

    Rapid evaluation method of inclusions in steel by use of cold crucible levitation melting has been developed. More than 70% of inclusions in steel were concentrated in surface layer of 70 μm thick by cold crucible melting in 5 min. Size distributions of alumina and slag type inclusions, and component of slag type inclusions were not remarkably changed by the fusion. X-ray fluorescence (XRF) with energy dispersive detection and fundamental parameter technique were employed to assess steel cleanliness rapidly. Indices of content could be obtained by XRF for alumina and slag type inclusions, respectively. Analytical time of 2.5 min was achieved when the sample was rotated during the measurement.

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  • © 2003 The Iron and Steel Institute of Japan

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