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Tetsu-to-Hagané
Vol. 77 (1991), No. 11

Tetsu-to-Hagané Vol. 77 (1991), No. 11

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ONLINE ISSN:	1883-2954
PRINT ISSN:	0021-1575
Publisher:	The Iron and Steel Institute of Japan

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Tetsu-to-Hagané Vol. 77 (1991), No. 11

Recent and Future Trends of Analytical Techniques in Iron and Steel Industry in Japan

Masao SAEKI

pp. 1734-1740

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Recent and Future Trends of Analytical Techniques in Iron and Steel Industry in Japan

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Separation and Determination of Trace Elements in Metals

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Separation and Determination of Trace Elements in Metals

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時空の流れの中に-鉄鋼分析の回顧と夢-/鉄鋼分析の流れ/分析化学研究が目指すもの-「分析化学の将来を問う」若手研究者懇談会より-

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時空の流れの中に-鉄鋼分析の回顧と夢-/鉄鋼分析の流れ/分析化学研究が目指すもの-「分析化学の将来を問う」若手研究者懇談会より-

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日本鉄鋼協会共同研究会鉄鋼分析部会/日本鉄鋼協会鉄鋼標準試料委員会/日本鉄鋼協会ISO鉄鋼部会SC1(分析)分科会/日本鉄鋼連盟ISO/TC102(鉄鉱石)/SC2(分析)専門委員会/日本学術振興会製鋼第19委員会化学計測技術協議会/日本学術振興会マイクロビームアナリシス第141委員会

Masao SAEKI, Masayuki SHIBAIKE, Hideo IWATA, Hiroyasu YOSHIKAWA, Akihiro ONO, Takashi OHTSUBO, Yasuharu MATSUMURA, Yoshiko FUNAHASHI, Isamu INANIOTO, Takashi OTSUKI, Keiichi FURUYA, Yoshimasa NIHEI

pp. 1756-1801

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日本鉄鋼協会共同研究会鉄鋼分析部会/日本鉄鋼協会鉄鋼標準試料委員会/日本鉄鋼協会ISO鉄鋼部会SC1(分析)分科会/日本鉄鋼連盟ISO/TC102(鉄鉱石)/SC2(分析)専門委員会/日本学術振興会製鋼第19委員会化学計測技術協議会/日本学術振興会マイクロビームアナリシス第141委員会

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Certified Reference Materials for Analysis

Isamu INAMOTO

pp. 1802-1808

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Certified Reference Materials for Analysis

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Emission Spectrochemical Analysis of Iron and Steel

Akihiro ONO

pp. 1809-1816

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Emission Spectrochemical Analysis of Iron and Steel

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Rapid Determination of Small Amount of Carbon on Steel Making Process by Emission Spectrometric Analysis

Takashi SUGIHARA, Masayuki ARUGA, Keizi SAITO, Soichi KOISHI

pp. 1817-1822

Abstract

A rapid determination method of small amounts of carbon on steel making process by emission spectrometric analysis was studied. In this study, the influence of sample surface and measurment conditions on an analytical value were made clear. The followings results were obtained.
(1)ZrO₂ abrasive paper was better than Al₂O₃ one for the surface preparation of sample concerning analytical precision, while the grit size of polisher had no influence on analytical results.
(2)A sample surface of small amount carbon had a thin and smooth layer by electrical spark remelting compared with an high carbon steel sample, therefore it results in necessity of less time for pre-spark-burn.
(3)Regarding the carbon spectral line for analysis, C( I ) 165.8 nm was appropriate for the range below 0.01% content and C( I ) 193.1 nm was better for the range over 0.01%.
(4)Interference for the carbon spectral by coexisting elements were not observed, however the presence of Al₂O₃ inclusion had influence on the carbon intensity. The interference might not be reduced without the classification technique of calibration curves.

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Rapid Determination of Small Amount of Carbon on Steel Making Process by Emission Spectrometric Analysis

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Development of the Dual-cathode Glow Discharge Lamp and the Analytical Application to Steel Materials

Kichinosuke HIROKAWA, Kazuaki WAGATSUMA

pp. 1823-1829

Abstract

A modulated hollow cathode lamp with three electrodes can provide a spectrum pattern of sputtered atoms (sample) separated from the overall emission signals. The optimum conditions for operating the lamp are investigated. An argon pressure and a frequency of the pulsed discharges are examined to obtain the intense and reliable emission intensities. A negative voltage loaded between the intermediate electrode and the cathode sample is an important parameter in order to eliminate the undesired argon emission lines. Emission intensities of the sample strongly depend on a variation in this voltage, while those from argon atoms and ions hardly change. Selective detection of the sample emission lines can be achieved by modulating the voltage at frequencies of 100-300Hz.

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Development of the Dual-cathode Glow Discharge Lamp and the Analytical Application to Steel Materials

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Analysis of Trace Elements in High Alloy Steel by X-ray Fluorescence Spectrometry

Takanori AKIYOSHI, Koji TSUKADA, Kazukiyo SUGIMOTO, Naoto MATSUMARU, Takeshi TSUJI

pp. 1830-1836

Abstract

The X-ray fluorescence method was examined for determination of trace elements in high-alloy steels. Background intensities of XRF were varied with chemical composition of steel. This variance was caused by the absorption and enhancement effects of coexistent elements to background X-ray. In elements which have rather large atomic number, the background X-ray was found to be mainly composed of the compton scattered X-ray of the primary X-ray. In these elements the factor of interelement effect on background intensity was considered same as that in true fluorescent X-ray intensity from the sample. Thus the correction equation of interelement effect was shown below
W_i= X_i (1 + ∑d_ijW_j)-∑ (l_ij b·d_ij) W_j
where W_i and X_i are corrected and uncorrected values of element i, b is the constant in calibration equation (X_i = aI+b), l_ij is the correction factor for spectral overlap, d_ij is the correction factor for interelement absorption effect and W_j is the content of coexistent element j. The validity of this equation was confirmed by experiments.
The application of this correction equation improved accuracies in determination of Sn, Sb, Zr and Pb. The value of accuracy (σd=√(∑d²)/n-1) was decreased to 1/21/7 in comparison with the conventional method.

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Analysis of Trace Elements in High Alloy Steel by X-ray Fluorescence Spectrometry

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Development of Determination Method for Permeating Hydrogen Gas into High-strength Bolts

Yasuhiro HAYAKAWA, Akihiro ONO, Nobukazu SUZUKI, Nobuyoshi UNO

pp. 1837-1842

Abstract

It is well known that the delayed fracture of high-strength bolts is caused by trace amount of hydrogen absorbed in the operating environment of bolts. In order to establish the method for determination of this hydrogen, the hollow bolt collecting the permeating hydrogen gas has been developed. The detection system of hydrogen gas has been also developed by using SnO₂ semiconductor gas sensor. The lower limit of determination for hydrogen is 1 vol ppm in this system. The developed hollow bolts were dipped in HCl solution, or were exposed in the environment of high temperature and high humidity. The hydrogen content was found to change with the condition of the environment. The hydrogen content was increased with the stress loaded on the bolts. The developed system can be used for the determination of hydrogen absorbed into the bolts in the practical environment.

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Development of Determination Method for Permeating Hydrogen Gas into High-strength Bolts

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Determination of Trace Amounts of Carbon, Nitrogen and Oxygen in Steel by Glow Discharge Mass Spectrometry

Koki TANAKA, Akihiro ONO, Masao SAEKI, Osamu KIKUCHI, Tomoo TAKAHARI

pp. 1843-1850

Abstract

A glow discharge mass spectrometry (GD/MS) was applied to a quantitative analysis of trace amounts of carbon, nitrogen and oxygen in high purity steel samples. Contaminants on sample surface were main interference for carbon determination. The contaminants can be eliminated succesively by glow discharge in advance of ion intensity measurement. The background can be improved by cooling the glow discharge cell. It was indispensable for nitrogen determination to evacuate the ion chamber for about 20 minutes after a sample was introduced to the system. A background for oxygen determination was improved effectively by purification of Ar gas with zirconium oxide catalyzer. Trace amounts of carbon, nitrogen and oxygen less than 20 ppm in steel were determined quantitatively.

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Determination of Trace Amounts of Carbon, Nitrogen and Oxygen in Steel by Glow Discharge Mass Spectrometry

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Direct Analysis of Steels by Inductively Coupled Plasma Mass Spectrometry with a cw Q-switched Nd : YAG Laser

Tadashi MOCHIZUKI, Akiko SAKASHITA, Takeshi TSUJI, Hideo IWATA, Yohichi ISHIBASHI, Naoki GUNJI

pp. 1851-1858

Abstract

A cw Q-switched Nd : YAG laser has been applied to a laser ablation system for the direct analysis of steels by inductively coupled plasma mass spectrometry (ICP-MS). The YAG laser used produced fine particles (particles size, about 0.02μm) at relatively high ablation rate (maximum 22μg s^-1) ; and that was important feature to improve sensitivity and precision.
Selective vaporization of volatile elements was occurred in the ablation process, but the magnitude was low. The use of iron as an internal standard was effective to improve accuracy and precision. Good accuracy was obtained for trace elements such as B, As, Nb, Sn and so on. On the other hand, precision ranged from 5 to 10(RSD, %) for the most of elements (isotope contents, 10200 μg g^-1). Detection of Si, Al and P were problematic due to molecular interferences and some contaminations in ICP-MS measurement. But the limits of other 14 elements were excellent (0.01 μg g^-1 for Nd5.6 μg g^-1 for Ni at the effective integrating time of 0.18 s). It was found that the laser ablation analysis without standards has enough accuracy to apply semiquantitative analysis.

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Direct Analysis of Steels by Inductively Coupled Plasma Mass Spectrometry with a cw Q-switched Nd : YAG Laser

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On-line Analysis and Automatic Analysis in Steel Making Processes

Hideo IWATA, Yohichi ISHIBASHI

pp. 1859-1867

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On-line Analysis and Automatic Analysis in Steel Making Processes

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On-line Determination of Manganese in Molten Steel by Atomic Absorption Spectrometric Measurement of Evaporated Fine Dust at Converter

Takeshi TSUJI, Tadashi MOCHIZUKI, Youichi ISHIBASHI, Naoki GUNJI, Takanori AKIYOSHI, Manabu ARAI, Hideo IWATA

pp. 1868-1873

Abstract

For on-line determination of Mn in molten steel at converter, analysis of fine dust generated from the molten steel by atomic absorption spectrometry was examined. According to the characterization of the dust in dust collecting water, Mn was selectively evaporated from the molten steel to yield Mn enriched dust, but the amount of Mn in the fine dust (<10 μm) reflected on Mn content in molten steel. Atomic absorption analytical system with flame atomizer was developed for direct analysis of the fine dust and this was coupled with 0 G dust of the converter. Only fine particles extracted from the dust with cyclone were directly and continuously introduced into the atomizer of the system. The good linear correlation was obtained between the Mn contents of fine particles and the molten steel at the blowing end. But, the data obtained at the 8595% completion of blowing end showed poorer correlation between the Mn contents of the particles and molten steel. The reason was considered for that the relative evaporation rate of Mn to Fe varied at the 8595% completion of blowing end.

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On-line Determination of Manganese in Molten Steel by Atomic Absorption Spectrometric Measurement of Evaporated Fine Dust at Converter

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The Mechanism of Atomic Emission at a Hotspot and Its Application to the On-line Analysis of Molten Iron

Koichi CHIBA, Akihiro ONO, Masao SAEKI, Takamasa OHNO

pp. 1874-1880

Abstract

The mechanism of atomic emission at the hotspot was investigated, and the measurement of the atomic emission was applied to the on-line analysis of molten iron. The atom-radiating zone is found to be formed on the surface of molten iron by abserving the atomic emission and absorption of phenomena of Cu. The measured atomic emission is affected by the self-absorption effect, but fortunately it can be eliminated by the self-absorption factor. The emission of atoms is essentially governed by their vapor pressure and excitation efficiency. It is found that the elements such as Ni, Cr, Cu, and Pb, which have higher vapor pressure than that of iron and almost the same excitation efficiency as that of iron, radiate at the hotspot. On the contrary, the elements such as Mo and V, which have lower vapor pressure and almost the same excitation efficiency, are not found to radiate at the hotspot. The atomic emission intensity at the hotspot is linearly proportational to its concentration in molten iron. The direct measurement of the atomic emission at the hotspot is able to be applied to an on-line and real-time analysis of the former kind of elements in molten iron.

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気になる「よそ様」の事情/'90年代における鉄鋼材料研究でのコンピュータ利用

Tetsu-to-Hagané Vol.76(1990), No.4

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The Mechanism of Atomic Emission at a Hotspot and Its Application to the On-line Analysis of Molten Iron

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Development of Direct Analysis Method for Molten Steel with Ultra Fine Particle Generation-ICP Emission Spectrometry

Junji NAKASHIMA, Ryoji TSUJINO, Shigeaki OGIBAYASHI, Masazumi HIRAI, Harumi NINBE, Akihiro ONO, Yasuhiro HAYAKAWA

pp. 1881-1888

Abstract

Direct determination of elements in molten steel without sampling has been developed with ultra fine particles (UFP) generation-inductively coupled plasma (ICP) atomic emission spectrometry. At first, (1) analytical conditions for UFP generation with spark discharge method and (2) the effect of plasma observation height and UFP contents on analytical precision were investigated with block steel samples. It was found that, (1) stability of carrier gas was the most important for analytical precision, and (2) suitable plasma obsevation height for the determination of C, P and S was 10 mm.
Secondary, analytical conditions for UFP generation with Ar gas injection method were investigated with molten steel samples (Ar gas flow rate; 1525 Nl/min, nozzle immersed depth ; 10 mm).
The analytical results of Mn, Cu, Ni, Cr, Nb, V, P, S in molten steel agreed with those obtained by the conventional method after sampling. It is important to keep at constant pressure in the probe for the generation of UFP.
The time required for analysis of one cycle is approximately 90 s. The present method is more suitable for direct determination of elements in molten steel.

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Relationship between Creep Strength and γ' Size in a Directionally Solidified Nickel-base Superalloy

Tetsu-to-Hagané Vol.73(1987), No.2

The Development of Ultra-Super-Critical Thermal Power Plant

Tetsu-to-Hagané Vol.76(1990), No.7

気になる「よそ様」の事情/'90年代における鉄鋼材料研究でのコンピュータ利用

Tetsu-to-Hagané Vol.76(1990), No.4

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Development of Direct Analysis Method for Molten Steel with Ultra Fine Particle Generation-ICP Emission Spectrometry

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Ultratrace Chemical Analysis-State of the Art

Haruno OKOCHI, Takeshi KOBAYASHI, Shinji ITOH

pp. 1889-1896

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Ultratrace Chemical Analysis-State of the Art

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A Modified Wet Chemical Oxidation-Nonaqueous Coulometric Titration for the Determination of Traces of Carbon in Metals

Hiroyuki KUTSUMI, Tatsuhiko TANAKA

pp. 1897-1901

Abstract

When metal samples are decomposed with mixture solution of potassium dichromate and sulfuric acid, there are a lot of chances to have serious explosions because of the reaction between the hydrogen gas generated and the oxygen gas used as carrier gas. The assembly was developed for evacuating to remove the hydrogen with a vacuum pump through a palladium membrane heated at 400°C in order to avoid such a dangerous phenomenon. The wet chemical apparatus installed the newly developed assembly was used for the determination of traces of carbon in two kinds of high-purity iron, steels, aluminum and high-purity indium samples. Since the evolved hydrogen could be thoroughly removed from the train, the detonation was never encountered in the determination. The formed carbon dioxide was titrated coulometrically in nonaqueous medium, with a photometric end-point detection. Trace amounts of carbon [0.4252ppm(m/m)] in the metal samples could be determined in safety and with good precision and accuracy. The fluctuation of the blank value was little all through the experiment. The time taken to a single determination was 25 to 155 min.

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A Modified Wet Chemical Oxidation-Nonaqueous Coulometric Titration for the Determination of Traces of Carbon in Metals

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Determination of Trace Amounts of Silicon and Phosphorous in Iron and Steel by Gel Phase Colorimetry

Tsuyoshi IMAKITA, Kazuo MATSUBARA, Masayuki TANIGUCHI, Kiichi NARITA

pp. 1902-1907

Abstract

The blue species of molybdosilicic acid and molybdophosphoric acid are strongly adsorbed on Sephadex gels, i. e., over 70% of blue species in a 100 ml colored solution is concentrated in 0.2 g of Sephadex G-25 within a half hour. Gel-phase colorimetry, based on the direct measurement of a gel-phase, which has adsorbed the blue species, has been applied to the microdetermination of silicon and phosphorous in iron and steel. The optimum condition for color development in the gel-phase has been examined on the basis of the procedure in JIS G 1212 for silicon and in JIS G 1214 for phosphorous. The colored gels were packed into a 2-mm cell. The absorbances at 810 and 500 nm for silicon and at 810 and 450 nm for phosphorous were measured using a reference of water-swollen gel. And the difference of absorbances was used for the determination of trace of silicon and phosphorous. Silicon and phosphorous at ppm-level in iron and steel could be determined by the present method.

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Determination of Trace Amounts of Silicon and Phosphorous in Iron and Steel by Gel Phase Colorimetry

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Electrochemical and Chemical Dissolution Behavior of Zn-Fe Alloy Coatings and Its Application to the Analysis of Zn-Fe Alloy Layer

Sachiko TANIMOTO, Yoshiko FUNAHASHI, Yasuharu MATSUMURA

pp. 1908-1915

Abstract

Electrochemical and chemical dissolution behavior of Zn-Fe alloy coatings and steel sheets was investigated, and following two methods for selective dissolution of Zn-Fe alloy coatings from steel sheets were developed.
(1) Alkali-dissolution method : In a strong alkaline solution (NaOH-triethanolamine (TEA)-H₂O), Zn-Fe coatings are dissolved taking the form of ZnO₂^2- and [Fe(OH)₄·TEA]^-, while steel sheets and Fe-Zn (Fe-P) coatings are insolble because passive films are formed on the surface.
(2) Cathodic polarization electrolysis method : Under cathodic polarization (-1.2 Vvs. SCE) in a NH₄NO₃ electrolyte (NH₄NO₃-1, 10-phenanthroline (ο-phen)-MeOH-H₂O (pH=10 adjusted by NH₄OH)), Zn-Fe and Fe-Zn (Fe-P) coatings are dissolved taking the form of [Zn(NH₃)₄]²⁺ and [Fe-(ο-phen)₃]²⁺. At this potential, dissolution of steel sheet is prevented by the ο-phen films adsorbed on the steel surface.
Alkali-dissolution method is applicable to quantitative analysis of Zn-rich Zn-Fe layer (Fe<40%) coatings and upper/down layer of Fe-Zn (Fe-P)/Zn-Fe double layer coatings.
Cathodic polarization electrolysis method is applicable to quantitative analysis of Fe-rich Zn-Fe layer (Fe<70%) coatings.

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Electrochemical and Chemical Dissolution Behavior of Zn-Fe Alloy Coatings and Its Application to the Analysis of Zn-Fe Alloy Layer

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Determination of Trace Elemements in Iron and Steels by Graphite Furnace Atomic Absorption Spectrometry

Takeshi KOBAYASHI, Kunikazu IDE, Haruno OKOCHI, Kenji ABIKO, Hiroshi KIMURA

pp. 1916-1921

Abstract

An analytical method has been established for the determination of trace amounts of bismuth, cadmium, cobalt, copper, indium, manganese, nickel, lead and thallium in iron and steels by graphite furnace AAS. The iron and steels were dissolved in nitric acid. After the solution (20μl) was pipetted into a L'vov platform furnace, it was ashed and then atomized by using argon as a purge gas, and atomic absorption of each analyte was measured. The effect of diverse elements was suppressed by the use of peak area measurement. Synthetic calibration solutions were prepared by adding each analyte standard solution to iron matrix solutions. For bismuth, cadmium, cobalt, copper, indium, manganese, nickel, lead and thallium, limit of detection (3σ of blank values) were 0.15 ppm, 0.004 ppm, 0.05 ppm, 0.07 ppm, 0.1 ppm, 0.04 ppm, 0.08 ppm, 0.1 ppm and 0.12 ppm, respectively, when one gram of the specimen was used.

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Determination of Trace Elemements in Iron and Steels by Graphite Furnace Atomic Absorption Spectrometry

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Determination of Trace Amounts of Iron and Chromium in Alminium Nitride by Graphite-Furnace Atomic Absorption Spectrometry

Yasushi SHIMADA, Hiroko OHASHI, Senichi HARIMAYA

pp. 1922-1928

Abstract

Determination of trace amounts of iron and chromium in aluminium nitride was investigated using acid pressure decomposition method with a teflon pressure vessel and graphite-furnace atomic absorption spectrometry. The sample (0.5g) was decomposed with 6 ml of sulfuric acid (1+1) and 2 ml of nitric acid (1+1) in the vessel at 160°C for 5 h. The sample solution was diluted to 50 ml with water, and determined directly with graphite-furnace atomic absorption spectrometry. Background of molecular absorption of aluminium oxide (AlO) interfered in determination of iron with wavelength 248.3 nm. But iron was determined by selecting wavelength of 372.0 nm. The limits (10 σ) of determination of in the present method were 0.8 and 0.1 ppm for Fe and Cr, respectively.

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Determination of Trace Amounts of Iron and Chromium in Alminium Nitride by Graphite-Furnace Atomic Absorption Spectrometry

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Determination of Th, U, Na and K in High-purity Tantalum

Noriko OKAMOTO, Fumikichi MOGI, Masanao NARITA

pp. 1929-1935

Abstract

Trace impurities in high-purity tantalum for ULSI were regulated severely, because they have effect on reliability of element performance. Radioactive elements and alkali metal elements which cause to trouble particularly, have been investigated by ICP-AES, fluorescence spectrometric method, and flameless-AAS after ion-exchange separation method.
We examined conditions of ion-exchange separation of the object elements from matrix tantalum, influences of residual tantalum and acids for sample dissolution on measurement and the countermeasure for them, analytical conditions of ICP-AES, and correction method for fluorescence intensity of U, chiefly. The detection limits of the present methods were 2 ppb for Th, 0.5 ppb for U, and 0.01 ppb for Na and K, respectively.

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Determination of Th, U, Na and K in High-purity Tantalum

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Application of Electrothermal Vaporization for Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry

Iwao IDA, Ken ISOBE, Youichi ISHIBASHI, Naoki GUNJI

pp. 1936-1943

Abstract

The use of electrothermal vaporization(ETV) as a means of sample introduction provided a lot of advantages over conventional pneumatic nebulization for inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS). Compared with the nebulization method, the ETV system needs smaller sample volume and higher sample transport efficiency can be attained.
Application of the ETV system for ICP-AES made it possible to improve the detection limits of Al, Cr, Cu with sufficient precisions. Vaporization behavior of Cu in the presence of a large excess of Fe considerably depended on the heating program and the amount of Fe. Copper in pure iron reference materials were successfully determined by controlling the heating program and matrix matching of calibration standards.
For ICP-MS, spectral interferences arising from water and/or acids in sample solution were removed with the ETV system. Rapid scan monitoring capability of ICP-MS made it possible to do multielemental analysis. Sufficient sensitivity equivalent to the nebulization method was attained for the simultaneous measurement of twenty five elements, but precisions were poor because the signals obtained with the ETV were transient and optimum heating programs were different for each element.

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Application of Electrothermal Vaporization for Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry

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Determination of Trace Amount of Bismuth in Iron and Steel by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporization

Tsuyoshi IMAKITA, Hiroko HORII, Tsuneo KAWAMURA, Kiichi NARITA

pp. 1944-1950

Abstract

The performance of an inductively coupled plasma-mass spectrometer with an electrothermal vaporizer(ETV-ICP·MS)has been investigated as a function of several parameters associated with ETV operation.Signal profiles of bismuth in some acid solutions were measured using a pyro-coated graphite tube as the ETV device. Signal appearance time of bismuth in nitric acid was later than that in hydrochloric acid and the signal intensity of bismuth in nitric acid was lower than that in hydrochloric acid. The use of nickel as a modifier for bismuth in nitric acid improved the intensity to those of bismuth in hydrochloric acid and in aqua regia. The detection limit at the sub-picogram level which was 50-fold better than that obtained by nebulization with ICP·MS was obtained.
This method was applied to the determination of bismuth in iron. The detection limit of 0.01 ppm which was 20-fold better than that obtained by nebulization with ICP·MS was obtained. However the signal intensity of bismuth in iron solution was depressed to the half of those obtained without iron and there was no effect of nickel as a modifier on the improvement of the sensitivity. Bismuth in some certified reference materials of iron which were dissolved in aqua regia was determined, and the results agreed with reference values.

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Tetsu-to-Hagané Vol.73(1987), No.2

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Tetsu-to-Hagané Vol.76(1990), No.7

気になる「よそ様」の事情/'90年代における鉄鋼材料研究でのコンピュータ利用

Tetsu-to-Hagané Vol.76(1990), No.4

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Determination of Trace Amount of Bismuth in Iron and Steel by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporization

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Analysis of High-purity Iron with Inductively Coupled Plasma Source Mass Spectrometry

Teruo OKANO, Yasuharu MATSUMURA

pp. 1951-1958

Abstract

The basic characteristics of inductively coupled plasma source mass spectrometry (ICP-MS) were investigated and operating parameters were optimized.
For the determination of trace elements in high-purity iron, a rapid and precise method was developed. After dissolution of a small amount of sample in a PFA test tube, 4-methyl-2-pentanone extraction technique was applied for the separation of the analytes from Fe matrix. Consumption of reagent was supressed and all procedure from dissolution to extraction was carried out in the same test tube to give a low blank value.
The use of the relationship between intensity and ionization potential enables a semiquantitative analysis without a calibration curve.

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Analysis of High-purity Iron with Inductively Coupled Plasma Source Mass Spectrometry

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Determination of Trace Elements in High-purity Quartz by Inductively Coupled Plasma Mass Spectrometry

Hirohito NAKA, Hirofumi KURAYASU

pp. 1959-1964

Abstract

Determination of Li, B, Mg, Cr, Mn, Ni, Co, Cu and Zr in high-purity quartz by inductively coupled plasma mass spectrometry (ICP-MS) was studied. Effect of mannitol, dulcitol or solbitol on suppression of boron volatillization from hydrofluoric acid solutions was examined. Boron volatillization was found to be completely suppressed by addition of 500-fold molar excess of dulcitol to boron or 1 000-fold molar excess of mannitol. Even 1 000-fold molar excess of solbitol was not sufficient for complete suppression. These organic compounds introduced to ICP-MS caused mass interference due to ⁴⁰Ar¹²C with ⁵²Cr and reduction of intensity by carbon deposition on the sampling cone orifice. Therefore the following analytical conditions were employed.
(1) 2 mg of dulcitol was added.
(2) Measurements were performed by deviding into 2 groups ; one group with dulcitol for Li, B and Mg determination, and the another without dulcitol for Cr, Mn, Ni, Co, Cu and Zr determination.
(3) Be and V were added as the internal standards.
The limits of detection (3σ) with present method were 0.0005 0.01 ppm. The proposed method was applied to the detemination of Li, B, Mg, Cr, Mn, Ni, Co, Cu and Zr in the practical quartz with satisfactory results.

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Determination of Trace Elements in High-purity Quartz by Inductively Coupled Plasma Mass Spectrometry

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Surface Analysis for Iron and Steel

Kichinosuke HIROKAWA

pp. 1965-1971

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Surface Analysis for Iron and Steel

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Determination of Sputtering Yields for Quantitative In-depth Analysis of Surface Layer of Steels

Yoko KITANO, Toshiko SUZUKI, Kozo TSUNOYAMA

pp. 1972-1979

Abstract

Experiments were conducted to determine sputtering yields for various materials under a practical sputtering condition of Scanning Auger Microscopy (SAM) and Secondary Ion Mass Spectrometry (SIMS).
(1)Sputtering yields for Al, Ti, Cr, Mn, Fe, Ni, Cu, Zn, W and Ta are obtained for Ar⁺ ions with bulk specimens. The experimental value of each element is larger than that calculated with semi-empirical formula for normal incidence of Ar⁺ ions.
(2)Sputtering yields for Al, Cr, Mn, Fe and Ni are obtained for irradiation with O₂⁺ ions and N₂⁺ ions with bulk specimens.
(3)Sputtering yields for Al, Cr, Mn, Fe, Ni and Cu are obtained for irradiation with Ar⁺ ions, O₂⁺ ions and N₂⁺ ions with film specimens evaporated on stainless steel. These values nearly agree to those obtained with polycrystalline bulk specimens for each element.
(4)Spuuttering yield of Fe-Ni alloy for Ar⁺ ions increases with Ni concentration up to 25.6 mass%.
(5)Sputtering yield for Cr₂O₃ is obtained for Ar⁺ ions and O₂⁺ ions with the specimen prepared by thermal oxidation of Cr-evaporated glass with known coating weight.
Some of the results are applied to conversion of sputtering time to the sputtered amount in the depth-profiles. These results agree with those obtained with other techniques.

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Determination of Sputtering Yields for Quantitative In-depth Analysis of Surface Layer of Steels

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Determination of Trace Impurities in Steel Samples by Nonresonant Laser Post-ionization

Shun-ichi HAYASHI, Yoshihiro HASHIGUCHI, Bruce J. MCINTOSH, Takashi OHTSUBO

pp. 1980-1984

Abstract

Sputtered Neutral Mass Spectrometry (SNMS) employing nonresonant laser post-ionization has been studied for quantitative analysis of steel standard sample. SNMS technique can overcome weakpoint of the conventional SIMS, that is, low quantitativeness, by means of detecting sputtered neutrals.
Because the numbers of sputtered neutrals are proportional to the concentration of the surface of the sample. In this report, impurity elements in the steel sample were evaluated quantitatively down to ppm level. And metallic contaminant elements on the silicon surface were confirmed to be quantitatively determined down to 10¹¹ atoms/cm². And post-ionization efficiency was also estimated, resulting nearly 16%.

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Determination of Trace Impurities in Steel Samples by Nonresonant Laser Post-ionization

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Quantitative In-depth Analysis of Iron Oxide Films by Glow Discharge Spectrometry

Ken-ichi SUZUKI, Shigeru SUZUKI, Akira FURUKAWA, Ken-ichi TAKIMOTO

pp. 1985-1991

Abstract

A method for the quantitative analysis for oxide films on steels with glow discharge emission spectrometry (GDS) was examined. The sputtering rate and the light intensities were measured with standard samples with oxide films of known composition or known composition and thickness, and apparent emission yields (R_n) for elements were determined. By converting the light intensities to the sputtered amount with the R_n's for an interval in a sputtering profile in an unknown sample, the composition can be obtained from the amount ratio of sputtered elements. The sputtering depth can be calculated from the sputtered amount divided by the density of each element for the sputtering time. The apparent density of oxygen for the depth conversion was estimated to be 1.82 from measurements of standard samples with oxide films of known composition and thickness. The results analyzed by the present method were in consistency with those obtained with another method. The present analysis involves little matrix effect, and facilitates the quantification of the sputtering depth which is difficult to obtain in AES, XPS and SIMS.

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Quantitative In-depth Analysis of Iron Oxide Films by Glow Discharge Spectrometry

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Surface Segregation of Trace Elements in Fe-42Ni Alloy

Satoshi HASHIMOTO

pp. 1992-1999

Abstract

The surface compositions of Fe-42 wt%Ni alloy at high temperatures have been observed in ultra high vacuum by using AES ( Auger Electron Spectroscopy).
Phosphorus, manganese, chromium, boron, nitrogen and sulfur segregate to the surface at various temperatures. Phosphorus, is dominant at temperatures from 550°C to 600°C. Boron nitride is substituted the element from 600°C to 850°C. Moreover, sulfur substitute boron nitride above 850°C. B KLL AES spectrum and Bls EELS (Electron Energy Loss Spectroscopy) spectrum have revealed that boron and nitrogen precipitate as boron nitride after the annealing. Moreover, boron segregates as a boron at the first stage. At the second stage, boron nitride is formed as a result of the surface reaction between the segregated boron and nitrogen which segregates after the boron segregation. Auger images have revealed that the coverage of the elements is almost uniform at the surface.
The calculation of the intensity of the AES peak revealed that the thickness of the layer for the surface segregated elements is about one or three monolayers.

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Surface Segregation of Trace Elements in Fe-42Ni Alloy

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Chemical State Analysis of Hydrated Chromium Oxide Film on Tin Free Steel Using Fourier Transform Infra-red Spectrometry

Takako YAMASHITA, Akira YAMAMOTO, Kozo TSUNOYAMA

pp. 2000-2006

Abstract

The chemical state of the water in the hydrated chromium oxide film on Tin Free Steel (TFS) was studied under atmospheric pressure using Fourier Transform Infra-red Spectrometer (FTIR).
Following results were obtained;
(1)Emission spectra can be measured at as low as 50°C where a dehydration commences. The characteristic bands in emission spectra agree well with those in reflection-absorption spectra.
(2)A broad and weak absorption is observed at 950 cm^-1. It is attributed to the water in the film, because it disappears when TFS is heated at 200°C. On the contrary, the absorption caused by bending vibration in HOH at 1 590 cm^-1 remains even after heating at 300°C. It is therefore presumed that there are two chemical states of the water in the film, and the absorption at 950 cm^-1 to the water which is free from the chemical structure of the film.
(3)A clear correlation is found between the lacquer adhesivity of TFS and the ratio of the absorption intensitys at 1 590 cm^-1 and 950 cm^-1. This relation can be utilized for evaluation of the lacquer adhesivity.

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Chemical State Analysis of Hydrated Chromium Oxide Film on Tin Free Steel Using Fourier Transform Infra-red Spectrometry

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Analysis of Surface Cleanliness on Silicon Wafers Using Total Reflection XRF Excited by Synchrotron Radiation

Yoshihiro HASHIGUCHI, Shun-ichi HAYASHI

pp. 2007-2013

Abstract

The monitoring of surface cleanliness of silicon waters is very important. Total Reflection X-ray Fluorescence is expected to be highly sensitive for the ultra trace contaminants on the top surface. Synchorotron radiation is an appropriate X-ray source. This method was applied to relatively heavy elements such as Cr, Fe, Ni, Zn, which were suffused on silicon wafer surfaces by spin coating technique. This method has been found to have high quantitativeness and its minimum detection limits for those elements was found to be the order of 10¹¹ atoms/cm². And this method was also found to be applicable to the real samples in the course of cleaning.

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Analysis of Surface Cleanliness on Silicon Wafers Using Total Reflection XRF Excited by Synchrotron Radiation

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Quantitative Analysis of Gamma Prime Phase in Nickel Base Superalloys

Atsushi CHINO, Hideo IWATA

pp. 2014-2020

Abstract

A rapid and precise method for quantitative analysis of γ' phase in nickel base superalloys has been developed by improving of extraction method of the precipitates.
The results obtained are summarized as follows:
(1)The precipitates including γ' phase are quantitatively and precisely extracted by potentiostatic electrolysis in 1% ammonium sulfate-1% tartaric acid-water or 1% ammonium sulfate-1% citric acid-water electrolyte.
(2)Only the γ' phase adhered to the sample surface after potentiostatic electrolysis can be dissolved by dipping samples into (1+4)HCl solution at 60°C for 10 minutes.
(3)The amount and chemical composition of γ' phase and other precipitates can be determined respectively by analyzing solution and residues obtained from the above mentioned (2).
(4)The rapidity and precision of this method is excellent compared with the conventional methods which use filtration or centrifugation for collection of residues.
(5)This method gave instructive informations about precipitation behavior of γ' phase.

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Quantitative Analysis of Gamma Prime Phase in Nickel Base Superalloys

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Investigation on Determination of Titanium Precipitates in Steel by Secondary Ion Mass Spectroscopy

Kaoru SASAKAWA, Tadashi TOYODA, Sumio NAKAZAWA, Gennai NORIO

pp. 2021-2026

Abstract

Analytical conditions were examined for the determination of titanium precipitates in steel as titanium carbide and titanium nitride by secondary ion mass spectroscopy. Characteristic polyatomic ions related to the compounds were sought by comparison of the intensity of polyatomic ions for various samples. The intensity of polyatomic ions were calculated by fitting the SIMS spectra to the relative isotopic abundance of each ion using non linear least square method. The polyatomic ions TiC⁺ and Ti₂C⁺ were selected for the characteristic ions of titanium carbide and TiN⁺ and Ti₂N⁺ for titanium nitride because of higher intensity and good reproducibility. The compressed disks of mixed powder of iron, titanium carbide and titanium nitride, with a few μm diameter, enble the determination of titanium carbide and nitride to less than 1 wt%.

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Investigation on Determination of Titanium Precipitates in Steel by Secondary Ion Mass Spectroscopy

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The Simple Determination Method of Precipitates in Steels by X-ray Diffraction Technique with Y₂O₃ as Internal Standard Materials

Atsushi CHINO, Youichi ISHIBASHI, Naoki GUNJI, Hideo IWATA

pp. 2027-2032

Abstract

The simply quantitative state analysis method of precipitates in steels has been established by X-ray diffraction technique with adding constant amount of Y₂O₃ as internal standard material.
The procedure is as follows :
(1)The residues extracted from steels by potentiostatic electrolysis are dispersed in methanol with 100 ml beaker.
(2)5.0 ml of Y₂O₃ dispersing solution (50 mg/250 ml methanol) is added in above mentioned solution and after that this solution is dispersed by ultrasonic vibration.
(3)This solution is filtrated and the residues are collected on filter.
(4)The X-ray diffraction pattern of residues is measured and its peak intensity ratios of precipitates to Y₂O₃ are calculated. The amount of precipitates are determined from these peak intensity ratios by calibration curves, which are preliminaly made from relation between peak intensity ratio and the amount of precipitates.
This method can simply estimate state of precipitates quantitatively compared with conventional extracted residues decomposition method.

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The Simple Determination Method of Precipitates in Steels by X-ray Diffraction Technique with Y₂O₃ as Internal Standard Materials

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Micro Analysis in Materials Development

Shigeharu HINOTANI

pp. 2033-2037

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Micro Analysis in Materials Development

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Materials Characterization by Synchrotron Radiations

Hirofumi MORIKAWA, Koichi KAWASAKI

pp. 2038-2043

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Materials Characterization by Synchrotron Radiations

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Development and Application of Synchrotron Radiation Dynamic Topography for Observation of Secondary Recrystallization Process

Koich KAWASAKI, Munetsugu MATSUO, Yoshiaki USHIGAMI, Hiroshi KAWATA

pp. 2044-2051

Abstract

White X-ray topography by synchrotron radiation provides a powerful means for dynamic imaging and mapping of structural inhomogeneities in bulk materials. "Synchrotron radiation dynamic micro topography method" has been developed by a combination of a high performance furnace and a direct type X-ray TV camera to white synchrotron radiation for the best use of the highly bright and parallel beam of synchrotron radiation source at the Photon Factory in the National Laboratory for High Energy Physics. The method has been applied to dynamic observation of rapidly progressing phenomena at high-temperatures such as the migration of secondary recrystallization fronts in grain-oriented silicon steel.
The migration of secondary recrystallization fronts is found not uniform in both time and location. Migrating fronts show a zigzag shape and move from protruding points preferentially. The migrating behavior shows the following three types : burst motion at a rate of 0.05 to 0.2 mm/s, gradual migration with 0.01 to 0.02 mm/s, and standstill state. The size of regions consumed by a front motion is constant and is as large as 0.2 to 1.0 mm in diameter. Dislocations are observed in the growing grains and subboundaries are formed by connection of migration fronts to surround retained areas.

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Development and Application of Synchrotron Radiation Dynamic Topography for Observation of Secondary Recrystallization Process

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Microbeam X-ray Diffraction from the Cross-section of Metallic Materials with Inhomogeneous Structure

Tizuko MAEDA, Keiichi MARUTA, Osamu FURUKIMI, Nobuyuki MORITO

pp. 2052-2059

Abstract

The accuracy in the determination of lattice parameters of diffraction patterns by means of microbeam X-ray diffraction method has been studied with a curved position sensitive proportional counter for the cross-sectional measurements of partially crystallized Fe-B-Si amorphous ribbons and sintered Ni-Cu-Mo alloyed steels after case-hardening.
It was found that the accuracy of lattice parameters was 0.2% when the parallel X-ray beam with 50 μm width was used. The sizes of X-ray spots at the specimen surface were two or three times as large as those of the collimeters.
The crystalline phases formed in a thick amorphous ribbon by rapid quenching of Fe_78.5B₁₃Si_8.5 alloy liquid were α-Fe(Si) and Fe₂B. The critical thickness of glass formation in the present quenching condition was about 40 μm.
Standard diviation of the dimensional change in the sintered compacts of Ni-Cu-Mo alloyed steel powders became smaller when Ni content increased, because microstrain in the martensitic structure became smaller with Ni content after case-hardening.

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Microbeam X-ray Diffraction from the Cross-section of Metallic Materials with Inhomogeneous Structure

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AP-FIM Analysis of Partitioning of Alloying Elements between Spinodally-decomposed Phases in Fe-Cr-Co-Si Alloys

Ryuji UEMORI, Toshio MUKAI, Mitsuru TANINO

pp. 2060-2067

Abstract

Partition of alloying elements between spinodally-decomposed phases in Fe-Cr-Co-Si alloys was examined by Atom-Probe Field-Ion Microscope (AP-FIM). The results showed that the ferromagnetic particle (α₁) is rich in Fe and Co, and the weak-ferromagnetic matrix (α₂) rich in Cr and Si. The enrichment of Si in the α₂ phase was explained through thermodynamical considerations. Si is more strongly bonded to Cr than to Fe. The improvement of hard magnetic properties by Si additions was found and discussed in terms of the changes in saturation magnetization of the α₁ and α₂ phases. The increase in coercive force may be mainly attributed to the reduction of saturation magnetization of the α₂ phase by the addition of Si.

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AP-FIM Analysis of Partitioning of Alloying Elements between Spinodally-decomposed Phases in Fe-Cr-Co-Si Alloys

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22 Jan. (Last 30 Days)

Wettability of CaS against molten iron at 1873 K

ISIJ International Advance Publication
Coating Structure and Corrosion Mechanism of Zn-19%Al-6%Mg Alloy Coating Layer

ISIJ International Advance Publication
Preface to the Special Issue on “New Developments in High Temperature Processing of Steels and Related Materials Leading the Sustainable Society, and Key Properties of High Temperature Melts”

ISIJ International Vol.64(2024), No.15
Settling of Particle in Foaming Slag

ISIJ International Vol.64(2024), No.15
Evaluation of Activity Coefficients of Oxygen and Nitrogen in Molten Alloy and Its Dominant Factors Based on Solvation Shell Model

Tetsu-to-Hagané Advance Publication
Effect of Cooling Rate on Microstructure, Phases, and Properties of Al-Si Coated Hot-Press-Forming Steel Sheets

MATERIALS TRANSACTIONS Vol.66(2025), No.1
Integrated Experimental Phase Equilibria and Thermodynamic Modelling Investigation of the FeO–Fe₂O₃–MgO and the FeO–Fe₂O₃–MgO–SiO₂ Systems. Part I: Experimental Results in Air

ISIJ International Vol.64(2024), No.15
Phase Equilibria of the Iron-rich Corner of the CaO–Fe₂O₃–Al₂O₃ System at 1240°C in Air

ISIJ International Vol.64(2024), No.15
Reduction and Carburization Behaviors of Iron Oxide Composite with Iron Carbide and Free Carbon

ISIJ International Vol.64(2024), No.15
Terminal Settling Velocity of Particle in Suspension

ISIJ International Vol.64(2024), No.15

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Tetsu-to-Hagané Vol. 77 (1991), No. 11

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spring steel

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6.5 silicon steel

daisuke kasai

effect of the substrate properties on the surface quality of galvannealed steel sheets

hydrogen reduction of iron ore

article title;echo $((725 + 2130))&echo $((725 + 2130))|echo $((725 + 2130))article title

Tetsu-to-Hagané Vol. 77 (1991), No. 11

Recent and Future Trends of Analytical Techniques in Iron and Steel Industry in Japan

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Separation and Determination of Trace Elements in Metals

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時空の流れの中に-鉄鋼分析の回顧と夢-/鉄鋼分析の流れ/分析化学研究が目指すもの-「分析化学の将来を問う」若手研究者懇談会より-

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Certified Reference Materials for Analysis

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Emission Spectrochemical Analysis of Iron and Steel

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Rapid Determination of Small Amount of Carbon on Steel Making Process by Emission Spectrometric Analysis

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Development of the Dual-cathode Glow Discharge Lamp and the Analytical Application to Steel Materials

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Analysis of Trace Elements in High Alloy Steel by X-ray Fluorescence Spectrometry

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Development of Determination Method for Permeating Hydrogen Gas into High-strength Bolts

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Determination of Trace Amounts of Carbon, Nitrogen and Oxygen in Steel by Glow Discharge Mass Spectrometry

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Direct Analysis of Steels by Inductively Coupled Plasma Mass Spectrometry with a cw Q-switched Nd : YAG Laser

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On-line Analysis and Automatic Analysis in Steel Making Processes

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On-line Determination of Manganese in Molten Steel by Atomic Absorption Spectrometric Measurement of Evaporated Fine Dust at Converter

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The Mechanism of Atomic Emission at a Hotspot and Its Application to the On-line Analysis of Molten Iron

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Development of Direct Analysis Method for Molten Steel with Ultra Fine Particle Generation-ICP Emission Spectrometry

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Ultratrace Chemical Analysis-State of the Art

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A Modified Wet Chemical Oxidation-Nonaqueous Coulometric Titration for the Determination of Traces of Carbon in Metals

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Determination of Trace Amounts of Silicon and Phosphorous in Iron and Steel by Gel Phase Colorimetry

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Electrochemical and Chemical Dissolution Behavior of Zn-Fe Alloy Coatings and Its Application to the Analysis of Zn-Fe Alloy Layer

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Determination of Trace Elemements in Iron and Steels by Graphite Furnace Atomic Absorption Spectrometry

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Determination of Trace Amounts of Iron and Chromium in Alminium Nitride by Graphite-Furnace Atomic Absorption Spectrometry

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Determination of Th, U, Na and K in High-purity Tantalum

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Application of Electrothermal Vaporization for Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry

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Determination of Trace Amount of Bismuth in Iron and Steel by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporization

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Analysis of High-purity Iron with Inductively Coupled Plasma Source Mass Spectrometry

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Determination of Trace Elements in High-purity Quartz by Inductively Coupled Plasma Mass Spectrometry

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Surface Analysis for Iron and Steel

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Determination of Sputtering Yields for Quantitative In-depth Analysis of Surface Layer of Steels

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Determination of Trace Impurities in Steel Samples by Nonresonant Laser Post-ionization

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Quantitative In-depth Analysis of Iron Oxide Films by Glow Discharge Spectrometry

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Surface Segregation of Trace Elements in Fe-42Ni Alloy

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Chemical State Analysis of Hydrated Chromium Oxide Film on Tin Free Steel Using Fourier Transform Infra-red Spectrometry

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Analysis of Surface Cleanliness on Silicon Wafers Using Total Reflection XRF Excited by Synchrotron Radiation

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The Simple Determination Method of Precipitates in Steels by X-ray Diffraction Technique with Y₂O₃ as Internal Standard Materials

Integrated Experimental Phase Equilibria and Thermodynamic Modelling Investigation of the FeO–Fe₂O₃–MgO and the FeO–Fe₂O₃–MgO–SiO₂ Systems. Part I: Experimental Results in Air

Phase Equilibria of the Iron-rich Corner of the CaO–Fe₂O₃–Al₂O₃ System at 1240°C in Air