Tetsu-to-Hagané
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ONLINE ISSN: 1883-2954
PRINT ISSN: 0021-1575

Tetsu-to-Hagané Vol. 60 (1974), No. 13

  • 「分析特集号」発刊にあたつて

    pp. 1727-1728

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  • An Expectation for Iron and Steel Analysis

    pp. 1729-1733

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  • 工業分析と日本学術振興会第19委員会

    pp. 1734-1739

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  • Report of the Joint Research Society of The Iron and Steel Institute of Japan

    pp. 1740-1740

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  • Report of the Iron and Steel Analysis Committee

    pp. 1741-1744

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  • Report of the Chemical Analysis Subcommittee

    pp. 1744-1752

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  • Report of the Photoelectric Emission Spectrochemical Analysis Subcommittee

    pp. 1752-1760

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    Readers Who Read This Article Also Read

    1. Amount of Aluminium Addition Required in Continuous Galvanizing Baths Tetsu-to-Hagané Vol.60(1974), No.1
    2. Relationship Between Austenitizing Time and Mechanical Properties of the Alloy Tool Steel SKD11 Tetsu-to-Hagané Vol.60(1974), No.1
    3. 焼戻脆性・高張力鋼 Tetsu-to-Hagané Vol.60(1974), No.4
  • Report of the Fluorescent X-ray Analysis Subcommittee

    pp. 1760-1763

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  • Report of the Nonmetallic Inclusion Analysis Subcommittee

    pp. 1763-1767

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  • Report of the Solid Masspectrometric Analysis Committee

    pp. 1767-1768

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  • Report of the Committee on Iron and Steel Standard Samples for Analysis

    pp. 1768-1777

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  • Chemical Analysis of Iron and Steel

    pp. 1778-1786

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  • Atomic Absorption Spectrochemical Analysis for Iron and Steel

    pp. 1787-1794

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  • Emission Spectrochemical Analysis of Iron and Steel

    pp. 1795-1798

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  • X-ray Fluoresdence Analysis of Iron and Steel

    pp. 1799-1804

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    Readers Who Read This Article Also Read

    1. 分析 Tetsu-to-Hagané Vol.57(1971), No.11
    2. 分析 Tetsu-to-Hagané Vol.57(1971), No.11
  • Gas Analysis of Iron and Steel

    pp. 1805-1819

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  • On Observation, Identification and Determination of Nonmetallic Inclusion and Precipitate in Steel

    pp. 1820-1826

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  • New Physical Methods in State Analysis

    pp. 1827-1842

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  • Automation of analysis of Iron and Steel

    pp. 1843-1853

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  • Analysis-Separation-Ecological Pollution

    pp. 1854-1861

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  • JIS System of Analytical Methods for Inon and Steel Industry

    pp. 1862-1868

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  • Application to Analysis of Microamounts of Gallium and Germanium in Steel by Using Quarternary Ammonium Salts

    pp. 1869-1878

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    Fundamental condition on isolation and determination of microamounts of gallium and germanium in iron and steel was carried out by means of quarternary ammonium salts and spectrophotometric methods.
    The procedure constitutes the preliminary separation of gallium and germanium from acid solution, addition of organic reagent, such as 4-(2-pyridilazo)-resorcine (PAR) or phenylfluorone, formation of complexes with quarternary ammonium salts to improve the color sensitivity.
    In gallium determination, the authors found that the water soluble gallium-PAR complex formed the ion-pair, which was extracted by chloroform, with zephiramine.
    The maxinum absorbance of the gallium-PAR-zephiramine complex in chloroform was at 513nm, and its molar extinction cofficient of the reaction was 1.07×105, and then 0.0003×0.05% of gallium in iron and steel could be determined in optimum condition.
    In germanium determination, the method by using cethyl trimethyl ammonium chloride (CTMAC) to germanium-phenylfluorone-complex was applied. The result showed that the germanium-phenylfluorone -CTMAC ratio was 1: 2: 2, and that 0.000×0.05% of germanium in iron and steel could be determination in optimum condition.
  • An Unusual Discharge Phenomenon and Its Effect on Pig Iron Analysis by Vacuum Emission Spectrometry

    pp. 1879-1891

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    In vacuum emission spectrometric analysis of pig iron by D. C. low voltage spark excitation in argon, an unusual or improper discharge, whose symptoms are a prolonged integration time and whitishlooking burn marks on the sample surface, is encountered on apparently good sound samples and gives seriously erratic results.
    The experiment showed that under the discharge in question the samples sparked with an integration time between 5 and 30% longer than normal and that the negative errors of 0.04% silicon, 0.025% manganese, and 0.02% phosphorus were common. The exception was sulfur but the results were less reproducible.
    An optical and electron microscopic study of the sample surface and burn marks revealed that the improper excitation was caused owing to a preferential sparking to flakes of graphite.
    A detailed study of the analytical conditions was carried out and it was found that a long pre-spark of 60 seconds altered the spark characteristics and improved the analytical accuracy and precision to a considerable extent.
    Some important problems associated with the spectrometry, i. e., the distribution of excited atoms in the analytical gap and the selection of internal standard lines, were also investigated and discussed.
  • The X-Ray Fluorescence Analysis of Oxide Materials by the Glass Bead Sample Technique

    pp. 1892-1899

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    An investigation has been made on the fluorescent x-ray analysis of oxide materials using the new glass bead technique and the correction coefficient for absorption and enhancement effects.
    Many publications on the glass bead technique have revealed that the breakdown or cracking of glass bead at the preparation has made the application of the technique limited in spite of its wider practicability.
    The results obtained are as follows:
    1) The fusion with use of anhydrous lithium tetraborate and a little amount of sodium bromide enables to get satisfactory glass beads without any strict annealing process to prevent the breakdown or cracking of them, and not to need particular crucibles such as made of Pt-Au to make the melt to be easily released. The addition of small amount of sodium bromide increase greatly the surface-tension of the fused melt and makes the melt release easily even from platinum crucible.
    2) The glase beads made by the anhydrous lithium tetraborate fusion are satisfactorily subjected to the fluorescent x-ray analysis, because they have flat and smooth surfaces and can be reserved for a long time without any change.
    3) By introducing the correction coefficients for absorption and enhancement effects, good agreement was observed between the wet chemical and the present fluorescent x-ray analytical methods for various oxide materials such iron making slags, mineral ores and welding fluxes.
  • Fluorescent X-ray Analysis of Iron Content in Iron Ores

    pp. 1900-1909

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    There has been problems on fluorescent X-ray analysis of iron contents in iron ores. It is the most important problem that the working curves of iron are different depending on the type of ore, such as hematite (Fe2O3), magnetite (Fe3O4), goethite (Fe2O3·H2O) and limonite (Fe2O3·nH2O), A theoretical calculation has revealed the reason for this effect. In the calculation, oxygen is considered an coexistent element and it is shown that the difference in coexistent elements cause the difference in Fekα fluorescent X-ray intensity of the same weight fraction of iron for various types of ore.
    Theoretical calculation were applied to the several types of ores and impurities and experimental results agreed well with the theoretical results.
    Theoretical correction method, interval standard correction method, and the dilution method with borax fusion and acid solution are also discussed theoretically.
  • X-Ray Fluorescence Analysis with Si (Li) Semiconductor Detector

    pp. 1910-1919

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    X-ray Fluorescence analysis sytem using Si (Li) non-dispersive detector is developed and it can be applied to steel industrial analysis. The system is especially suitable to the on-line rapid analysis as the Si (Li) detector has very high sensitivity and is not affected by circumstance. The applicatinos of the system are as follows.
    (1) On-line X-ray fluorescence analysis of tubings in order to distinguish the type of steel.
    (2) X-ray fluorescence analysis of particular shape objects, such as wire cross-section, large forged steel etc.
    (3) Thickness measurement of coating on steel sheet zinc coating thickness for galvanized sheet and paint thickness of colored galvanized sheet.
    (4) X-ray diffraction
    The results are very excellent, resolution power and stability are practically satisfied.
  • A Fundamental Study of Fluorescent X-ray Analysis for Analysis of Non-metallic Inclusions in Steel

    pp. 1920-1929

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    Non-metallic inclusions in steel are closely connected with quality of steel, and it is extremely important for the investigation of pecuriality and effects of added elements of steels to understand precipitated shapes, distribution and quantities of inclusion.
    In this report, the results of fundamental studies on determination of nonmetallic inclusions in steel by fluorescent X-ray analysis are described.
    In the experiments, non-metallic inclusions were isolated by hot nitric acid or iodire-methanol method, and which were supported on the suitable filters to be determined by the fluorescent X-ray analyzer Fluroprint MK-II The analyzed elements are Si, Al, Fe, Mn and Cr.
    The results were summarized as follows;
    (1) According to the surface observarion of filters, which were treated with NaOH solution (3%). by scanning electron microscope, Membran filter MF3O was found to be the most suiable as support for residues.
    (2) In the iodine-methanol method, the amorphous carbon is isolated with inclusions simultaneously and interferes in the fluorescent X-ray analysis. But the amorphous carbon can be removed from residues by ignition in Platinum cruciLle at a temperature below 400°C.
    (3) Fluorescent X-ray intensities of Si and Al are affected by Fe, Mn and Cr, but in the case of more than 200μg of Si or Al, effect of 1000μg of Fe+Mn is negligible.
    (4) As compared with general chemical analysis on Al2O3 inclusion in Al-killed carbon steel, average and standard deviation of difference were 0.0001% and 0.0006%.
  • Preparation of Sample for the Determination of Hydrogen in Ferroalloys

    pp. 1930-1934

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    On the determination of hydrogen in ferroalloys, values obtained are much influenced by analytical methods and conditions of sample preparation. The authors have examined about the powdered sample and granular sample by using method of heating in argon carrier gas and fusion in argon carrier gas or vacuum, in order to establish a suitable method on the determination of typical hydrogen content.
    The results obtained are as follows:
    (1) In the granular sample of Fe-Ti, lower values are obtained by method of heating in argon carrier gas because of difficulty in extracting hydrogen from sample. On the other hand, in the powdered sample under through a 16 mesh sieve, hydrogen can be extracted completely.
    (2) Hydrogen are not homogeneous in crushed sample of Fe-Mn, Fe-Si, etc. generally, hydrogen content in powder is much higher than that in granular and there are large differences in hydrogen content according to the positions (e. g. surface and core) of sample taken from the original block. Therefore it is desired to use powder sample mixed sufficiently after sampling homogeneously from crushed block in order to obtain a reliable values of hydrogen in ferroalloys.
    (3) Absorption of hydrogen does not occur during crushing of block or granular sample and exposure of powdered sample in room atmosphere.
    (4) Hydrogen values obtained by the fusion extraction method are much influenced by temperature of extraction at some kinds of alloys (e. g. Fe-V, Fe-Si). Therefore it is necessary to choose a suitable temperature according as composition.
  • Analytical Chemical Investigation of Sulfide of Rare Earth Elements in Steel

    pp. 1935-1943

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    In order to establish a method for phase analysis of rare earth elements in hot rolled steels, the chemical behavior of various compounds of rare earth elements, both synthesized and extracted from the steels, were investigated.
    The extraction of compounds of rare earth elements from the steels was carried out well by electrolysis in non-aqueous medium, and the extracts were found by X-ray diffraction to contain sulfide, oxysulfide (RE) 2O2S and/or oxide of rare earth elements.
    The procedure for phase analysis of rare earth elements in steel is as follows:
    (1) 0.5-2g of sample is electrolytically decomposed in 600 ml of methly alcohol containing 5% triethanolamine and 1% tetramethyl ammonium chloried at a current density of 50mA/cm2 under nitrogen atmosphere, and the extracted residue is filtered.(Separation of combined rare earth elements)
    (2) Amount of metallic rare earth elements is calculated by subtraction of combined rare earth elements fraction from the amount of total rare earth elements.
    (3) The extracted residue is then treated with the 50ml of I2-methly alcohol (10%) at room temperature for 30 min and filtered again.(Separation of oxy-sulfide and oxide of rare earth elements)
    (4) Amount of sulfide of rare earth elements fraction is calculated by subtraction of the amount of oxy-sulfide and oxide of rare earth elements fraction from the combined rare earth elements fraction.
    The method for phase analysis was applied to several hot rolled steels containing various amount of rare earth elements and sulfur.
    The result showed that the anisotropy (C/L) of impact values, the ratio of impact value normal to rolling direction and the one parallel to it under the same condition, is considerably effected by the yielding rtio (r) of sulfide of rare earth elements
    (r= S as RE sulfide/S as (Mn sulfide+RE sulfide)).
    The relation was observed to be approximately represented by the formula.
  • Study on Phase Analysis of Boron in Steel

    pp. 1944-1956

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    An attempt has been made to establish a method for phase analysis of boron in steels which contributes to investigation of hardenability.
    The experimental results obtained were as follows;
    (1) Extraction of boron compounds from steel was confirmed to qe favorably carried out by either the I2-CH3OH (14%) method or the electrolytic method.
    (2) It was also found that fine particles of boron compounds are apt to be dissolved by H2SO4 (1+6) at 60°C and a part of them passes through the filter paper containing a litile amount of filter pulp.
    (3) The strong phosphoric acid decomposition of sample is most suitable for determination of total boron in steel.
    (4) The effective boron is calculated by subtraction of the I2-CH3OH insoluble boron fraction from the total boron amount determined by the strong phosphoric acid method.
    (5) The effect of boron on hardenability of steel is observed to correspond evi iently with the effective boron content.
    (6) The investigation on boron distribution by means of the a-track technique suggested the relation between concentration of boron on pre-austenitic grain boundaries and the effective boron content.
  • Analysis of Titanium Carbide in Austenite Stainless Steel

    pp. 1957-1961

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    The favorable methods for isolation and determination of titanium carbide from austenite stainless steel added Ti were examined, and by use of these methods, solubility product constant of titanium carbide in austenite stainless steel was determined.
    The results were summarized as follows:
    (1) For the isolation titanium carbide from austenite stainless steel, constant current electrolytic method by use of 5% HCl methanol was recommended.
    (2) New combustion method for separative analysis of carbides in residue was studied and developed, by which, isolated residue was burned in pure O2gas stream at regulated temperature and CO2produced was determined by conductornetric method. And then amounts of carbides present in residue were found respectively.
    (3) Under some presumption, solubility product constant of titanium carbide in austenite stainless steel heat-treated 950°C-1200°C was examined, and logS=-7210/T+3.19 was obtained. Here S is the solubility product constant, and T is absolute temperature.
  • Fundamental Study on Isolation and Determination of Carbides in Steel

    pp. 1962-1979

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    Some mineral acid separation and potentiostatic electrolysis method for isolation and determination of various carbides in steels have been fundamentally investigated.
    The results obtained are summerized as given below.
    1. Globular and coarse Fe3C and other various carbides such as TiC, ZrC, VC, NbC, (Cr, Fe) 7C3, (Cr, Fe) 23C6, Mo2C and (Fe, W) 6C were extracted quantitatively by means of potentiostatic electrolysis method with 15% sodium citrate-1.2% KBr-30% citric acid or acethyl aceton-1% tetramethyl ammonium chlolide-methanol electrolyte.
    2. The reproducible separation of TiC, VC and NbC with HCl (1+1) and (Cr, Fe) 7C3, (Cr, Fe) 23C6and Mo2Cwith H3PO4 (2+1) could be successfully accomplished if these carbides were relatively coarse.
    3.TiC, ZrC and VC being considered insoluble in mineral acids were found to be attacked gradually by diluted HCl, H2SO4and H3PO3and were mare easily dissolved as the particles cf the carbide were fine.
  • An Ion Microprobe Mass Analyzer and its Application to Iron and Steel Research

    pp. 1980-1988

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    The application of an ion microprobe mass analysis to the study of iron and steel making processes was examined with Hitachi model IMA-2 ion microanalyzer (IMA) equipped with specific devices designed so as to meet the recent requirements in steel research: devices for sample heating, line analysis, step scanning and brittle fracture at low temperature together with photographic systems for the images by use of secondary ion, total ion, and secondary electron. Several examples of the application of ion microprobe mass analyzer to the study of iron and steel making processes are discussed with respect to the analysis of trace elements particularly at the surfaces fractured by hydrogen blistering and the grain boundary segregation. Ion microprobe mass analysis is expected to provide the more useful information which have never been known to date in the field of material science.
  • Application of Ion Microprobe Mass Analysis of Iron and Steel

    pp. 1989-2001

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    Application of secondary ion analysis to iron and steel was investigated by using the ion microprobe mass analyzer. The method of sample preparation was compared, and the surface polished with Al2O3powder was found to be the most suitable for in-depth analysis. This technique was applied successfully to the analysis of surface segregation of Al in Fe-0.1%Al alloys. Quantitative analysis of alloy elements in steels was investigated by both of calibration curves and the theore tical correction method called CARISMA. In low alloy steels, it was found to be possible to perform quantitative analysis with good accuracy by means of calibration curves. However, when the concentration of an alloy element in steel exceeded a certain value, the analytical value determined by ion probe microanalysis was sometimes fairly larger than that by chemical analysis. It was confirmed that the over estimation was caused by the formation of secondary phases, such as carbides, in the matrix. The analytical value determined by CARISMA was not so accurate as that by calibration curves, but the precision of this correction method was not influenced by the formation of secondary phascs.
  • Investigation on the Metallographic Analysis of Small Amount of Aluminium in Steel by Emission Spectroscopic Analysis

    pp. 2002-2012

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    In previous papers described for analysis of Al in steel by emission spectroscopy, the analytical values were affected mainly by the amounts of Al2O3 in the sample, the difference in a situation of the grinding of the sample surface and so on.
    For the elimination of these affections, a study has been carried out on the behaviors of integrated photo-current pulses occured from every unit discharge.
    As the result of many considerations, it was found that Al in steel has been able to be determined metallographically; Al as in the homogeneous state (acid-soluble Al at chemical analysis) and as in the inhomogeneous one (insoluble Al) respectively. The efficient and appropriate informations used to the metallographic analysis was derived from the distribution of integrated photo-current pulses.
    This distribution was obtained by the following techniques. The pulses occured from every unit discharge were shaped and amplified suitably and must be put through multi-channel pulse height analyzer circuit. After treatment in P. H. A., the output pulse amplitude shows the distribution due to the metallographical state of Al in the sample.
    The median value shows T. Al, and the shift of the median values during spark time show insol. Al in the sample, respectively.
    In this method, the results obtained are 0.0015% Al (δ)(at the range of 0-0.05% Al) for T. Al and 0.0018% Al (δ)(at 0-0.04% Al) for sol. Al respectively.
  • Infrared Spectroscopic Study of Al Oxides in Al-killed Steel

    pp. 2013-2017

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    Aluminium oxides produced by deoxidation process of steel were examined interms of ir. absorption spectroscopy. Theta or the analogous phase of Al2O3 was found generally in Al-killed steel.
    Absorption spectrum proves the tetrahedral sites in monoclinic Al2O3 are partially occupied by Al atom and the occupation probability ratio of tetrahedral site to octahedral site is not constant in deoxidized and killed steel by Al. The deoxidation product could be considered to be in the transitional structure from theta to alpha phase. Preliminary experiments show the theta crystal synthesized is partially soluble to acids compared with alpha-Al2O3. The solubility to acids may effect on the collecting yield of Al2O3 included in steel.
  • Automatic Chemical Analysis of Phosphorus and Boron in Steel

    pp. 2018-2026

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    The automatic analytical methods for boron and phosphorus in steels have been studied using Technicon Auto Analyser.
    The experimental results were as follows;
    (1) Phosphorus in steel was found to be automatically determined sucessfully by the adaptation of the established molybdenum-blue spectrophotometric procedures.
    When the iron content is Lelow 50%, however, the violent evolution of SO2 is caused by the remaining of much amount of sodium bisulfite which was not oxidized by ferric iron and makes it impossible to determine the phosphorus content due to the turbulence of the absorption curve.
    The time required for analysis of 20 samples was 3 hours and remarkably shortened as compared with that by the manual analysis (about 7 hours).
    (2) Boron in steel was found to be automatically determined successfullyby the adaptation of the established methylene-blue spectrophotometric procedures which involve thestrong phosphoric acid decomposition and the elimination of the interference from excess HF.
    The time required for analysis of 20 samples was 2 hours and remarkably shortened as compared with that by the manual analysis.
  • The Development of an Automatic Apparatus for Dissolving Samples and Its Applications to the Analysis of Steels

    pp. 2027-2034

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    To rationalize the analytical procedures, an automatic apparatus for dissolving steel samples was developed and applied to prepare the solutions for the instruments of solution analysis.
    The developed apparatus is composed of the devices for supplying chipped steel samples, adding the reagent solutions, dissolving by heating the solution, filtrating the prepared solution and storing the filtrates and precipitates.
    When weighted chipped steel samples are placed on the sample feeder, the apparatus prepares 74 solutions automatically in one night. This apparatus is able to be appliedto many dissolving methods with acids such as HCl, HNO3, HClO4 and capable of judging the dissolving conditions.
    The analysis of the solutions prepared by the apparatus were then carried out using the atomic absorption spectrophotometer, emission spectrometer and automatic solution analyzer. The results agreed with those obtained by the handwork.
    The application of the newly developed apparatus to the routine analytical work has shown a remarkable improvement in work.
  • Development of an Automatic Photometric Analyzer

    pp. 2035-2044

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    A new automatic photometric analyzer has been developed as a series of studies on automation of wet chemical analysis of iron and steel samples. The developed analyzer (Photo. 1, Fig. 1) performs automatically and continuously all the photometric procedures after preparation of sample sulution usually by acid dissolution method. The above procedures were previously carried out by complicated and time-comsuming manual operation.
    The analyzer is mainly composed of the injecting davice for sample solution, the adding device for reagent solutions and water, the device for developing color and measuring the absorbancy, the controlling device and the recording device. The third device is most characteristic and is composed of the reaction vessel and the solution circulating pipe with a gas blowing tube, a bubble eliminator, an absorbancy measuring cell and a drain cock.
    The analyzer was applied to determination of phosphorus, silicon, manganese and acid soluble aluminum in steel samples. From 0.0005% to 0.1% of phosphorus was determined in 6 min for one determination on principle of molybdenum blue spectrophotometry. From 0.002% to 1% of silicon was determined in 6 min on principle of molybdenum blue spectrophotometry. From 0.001% to 1% of manganese was determined in 5 min on priciple of sodium periodate oxidization spectrophotometry. From 0.0005% to 0.01% of acid soluble aluminum was determined in 6 min on principle of eriochrome cyanine R spectrophotometry.
  • Determination of Total Iron in Iron Ores by Titanium Trichloride Reduction-Organic Redox Indicator Method

    pp. 2045-2055

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    In order to prevent the poliution of the drain-age from a chemical labolatory by Hg, the authors proposed two new methods for the determination of total iron in iron ores in place of JIS method in which Fe (III) is reduced with SnCl2 and the excess of reductant is oxidized HgCl2. Those method are as follows:
    For the purpose of verification analysis we established TiCl3 reduction-ITS indicator method in which the most part of Fe (III) is reduced with SnCl2, the remaining reduced with TiCl3 and the excess of TiCl3 is oxidized with K2Cr2O7 using indigo tetrasulfonic acid as the indicator. Dissolution of sample and titration of Fe (II) are the same as JIS method.
    Cu (<2mg) and V (<3mg) do not interfere. Analytical results of iron ores by this method agreed closely with those by JIS method.(dmax=0.04%Fe)
    For the purpose of rapid analysis was established TiCl3 reduction-NR indicator method in which main reagents used are H3PB4+H2SO4, metallic Al and neutral red indicator in place of HC1, SnCl2and ITS indicator in the former method, respectively. Sn and V (>1.2mg) interfere. Analytical results of iron ores without interfering elements by the later are similar to the former.
  • Determination of Small Amounts of Oil in Waste Water

    pp. 2056-2061

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    An analytical method for down to 0.1 ppm of oil in waste water was studied and the recommended analytical procedure was presented. Small amounts of oil was found to be selectively absorbed by sericite powder and carbon of the powder absorbing oil was determined. Absorption method for small amounts of oil, effect of pH of sample solution and co-existing materials in the solution, analytical method for determination of carbon in the powder absorbing oil and oil itself and pretreatment of sample solution were studied and discussed in details. The recommended procedure is as follows.
    Sample solution (10-100 ml) is filtrated by Nuclepore filter (5μ) and washed by ethyl alcohol. The filtrate is mixed for about 1 min with 10 mg of sericite powder under ultrasonic agitation (40.5 KHz). The powder absorbing oil is separated by filtration with Nuclepore filter (1μ) and washed by water. The powder with the filter is dried at about 50°C. After the filter is removed, carbon of the powder absorbing oil is determined by the conventional combution carbon analyzer at the combution temparature of 900°C.
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