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WO1993007100A1 - Utilisation et selection de materiaux de revetement et de surface pour lutter contre l'encrassement et la corrosion de surface, par la mesure du potentiel zeta - Google Patents

Utilisation et selection de materiaux de revetement et de surface pour lutter contre l'encrassement et la corrosion de surface, par la mesure du potentiel zeta Download PDF

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Publication number
WO1993007100A1
WO1993007100A1 PCT/US1992/008238 US9208238W WO9307100A1 WO 1993007100 A1 WO1993007100 A1 WO 1993007100A1 US 9208238 W US9208238 W US 9208238W WO 9307100 A1 WO9307100 A1 WO 9307100A1
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WO
WIPO (PCT)
Prior art keywords
coating
candidate
fouling
potential
measuring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1992/008238
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English (en)
Inventor
Palitha Jayaweera
Samson Hettiarachchi
Howard Ocken
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Electric Power Research Institute Inc
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Electric Power Research Institute Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Electric Power Research Institute Inc filed Critical Electric Power Research Institute Inc
Priority to JP5506989A priority Critical patent/JPH06504093A/ja
Publication of WO1993007100A1 publication Critical patent/WO1993007100A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F15/00—Other methods of preventing corrosion or incrustation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/60—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrostatic variables, e.g. electrographic flaw testing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack

Definitions

  • This invention relates to the use and selection of coating and surface material to prevent fouling deposit formation on surfaces, using zeta potential measurement to select appropriate materials.
  • Electrokinetic phenomena involve either the movement of charged particles through a continuous medium or the movement of a continuous medium over a charged surface.
  • the four principal electrokinetic phenomena are electrophoresis, electroosmosis, streaming potential and sedimentation potential. These phenomena are related to one another through the zeta potential, , of the electrical double layer which exists in the neighborhood of the charged surface.
  • the distribution of electrolyte ions in the neighborhood of a negatively charged surface and the variation of potential, ⁇ , with distance from the surface are well known in the art (see, for example, Zeta Potential in Colloid Science - Principles and Applications; R.J.Hunter; Academic Press, N.Y. (1988) ) .
  • Two different layers of ions appear to be associated with the charged surface.
  • the layer of ions immediately adjacent to the surface is called the inner Hel holtz (IH) layer; the second layer of ions is the outer Helmholtz (OH) layer.
  • Ions of the IH layer are held to the charged surface by a combination of electrostatic attraction, specific adsorption forces and chemical bonds.
  • the thickness, ⁇ , of this* layer is assumed ⁇ - be equal to the ionic radius of the specifically adsorbed ionic species.
  • the second layer of ions is the OH layer.
  • the boundary between the two layers is the limiting inner Helmholtz plane.
  • the ions outside the OH layer are acted upon only by electrostatic forces andthermalmotions ofthe liquid environment (Brownian motion) , and they form a diffuse atmosphere of opposite charge to the net charge at the OH plane.
  • the net charge density of the ion atmosphere of the diffused layer decreases exponentially with distance from the limiting OH plane.
  • Thediffused layer forms one half of an electrical double layer, and the charged surface plus the inner and outer Helmholtz layers form the other half.
  • the effective distance of separation 1/k between the two halves of the double layer is determined by the concentration of electrolyte (ionic strength) .
  • concentration of electrolyte ionic strength
  • the relationship for 1/k from the Debye-Huckel theory is described by an equation.
  • C is the concentration
  • Z is the valency of the ionic species.
  • Variation of potential, , with the distance x from the charged surface decreases linearly with increasing distance x in the region of the inner and outer Helmholtz layers. In the region of the diffused layer, ⁇ decreases exponentially with increasing distance x.
  • q e is the charge on the particle.
  • 1/k is the effective thickness of the double layer
  • D the dielectric constant of the liquid
  • a the particle's radius at the plane of shear.
  • Equation 2 and 3 above show that the ⁇ - potential is determined by the net charge at the plane of shear and 1/k, the effective thickness of the ion atmosphere.
  • the ⁇ -potential controls the rate of transport between the charge surface and the adjacent liquid.
  • rate of transport v E and the f-potential which is valid for all four electrokinetic phenomena is given by a sixth equation, where v E is the velocity of the liquid at a large distance from the charged surface, E is the field strength (V/cm) , and ⁇ is the viscosity of the liquid.
  • Equation 6 The equations which relate f-potential to the streaming potential may be obtained from Equation 6 by use of Poiseuille's law for laminar flow through a capillary.
  • v E is the velocity of the particles.
  • E is the applied field strength for electrophoresis, whereas it is the gradient of potential developed by the sedimentation of charged particles in the sedimentation effect.
  • oxides are typically produced as corrosion products in the feedwater systems of commercial nuclear and fossil fuel power plants. Corrosion products deposited on surfaces involved in critical measurements can effect the reliability of those measurements. For example, such corrosion products deposited on critical surfaces of the Venturis that are used to measure mass flow rates in power plants will result in higher energy utilization and costs. Thus, it would be highly beneficial if coatings or surfaces could be discovered which have physicochemical properties whichwould in theoryrepel foulingmaterials of concern for a particular application, for example, the same sign of surface charge at the operating pHvalue as the charge of the oxide corrosion products; those substances likely will repel the fouling or corrosion products via electrostatic repulsion and thus prevent fouling or corrosion of the surface of interest.
  • FIGURE 1 shows theexperimental arrangementused for zeta potential measurement.
  • automated computer control of the measuring process is accomplished using components shown in the FIGURE and software developed to monitor and control the system.
  • FIGURE 2 is an enlarged and expanded view (central figure) of the rulon column section of the loop.
  • the substance or surface to be measured is held in place by platinum screens and, if necessary, tsflon filters as the electrolyte flows through and contacts the substance or surface.
  • FIGURE 3 shows the results of zeta potential measurement vs. pH at 235°C for Fe 3 0 4 .
  • FIGURE 4 shows the results of zeta potential measurement vs. pH at 235°C for the PdO.
  • FIGURE 5 shows results of zeta potential measurement vs. pH at 235°C for the W0 3 .
  • FIGURE 6 shows results of zeta potential measurement vs. pH at 235°C for the Fe 2 0 3 .
  • FIGURE 7 shows the results of zeta potential measurement vs. pH at 235°C for Fe 3 0 4 in solutions aerated for different periods.
  • FIGURE 8 shows results of zeta potential measurement vs. pH at 235°C for an actual foulingmaterial collected from the feedwater duct of a power plant.
  • FIGURE 9 shows results of zeta potential measurement vs. pH at 235°C for Ti0 2 .
  • FIGURE 10 shows results of zeta potential measurement vs. pH at 235°C for Ta 2 0 5 .
  • FIGURE 11 shows results of zeta potential measurement vs. pH at 235°C for NbjOj.
  • Fig. 1 The experimental arrangement for high temperature f-potential measurements is shown in Fig. 1 and in Fig. 2.
  • An electrolyte is pu_.pcd into the loop by a commercial HPLC pump 1.
  • the loop 2 is made of 1/4" and 1/8" stainless steel tubing.
  • Heating tapes 3 wrapped around the stainless steel tubing are controlled by commercial temperature controllers 4 that sense the temperature at both ends of the rulon column.
  • High temperature pH is measured with a yttria-stabilized zirconia (YSZ) pH electrode 5 and an external pressure balanced reference electrode (EPBRE) 6.
  • the pressure of the system is measured by a pressure gauge 7 and pressure is maintained by adjustable pressure release valve 8.
  • the solution is cooled to room temperature by passing it through a cooling jacket 9 before it is discharged from the system.
  • YSZ yttria-stabilized zirconia
  • EPBRE external pressure balanced reference electrode
  • the substances to be studied are packed into a rulon column 10 which is tightly fitted inside the stainless steeltubing 2.
  • Rulon provides the electrical isolation of the substance powder 11 from the stainless steel tubing wall. Powder is held in the column by Pt screens 12 that also serve as electrodes formeasuring streaming potentials. For very fine powders, teflon filters 13 are used in addition to Pt screens. Contacts to the electrodes are made through rulon ferrules 14.
  • the column region 10 of the loop is thermally well insulated to avoid heat losses and maintain the column at the required temperature.
  • Rulon columns 10 are made to different lengths such that they provide easily measurable pressure drops across the column. In a newer design, column lengths can be changed simply by changing the thickness of the center rulon ring 10.
  • the powder 11 is packed in the center opening of the ring and the three rings 10 are held tightly by pipe fittings that also provide the high pressure seal.
  • Nominal thicknesses of rings are about 3/32" for outer electrode holder rings and about 3/16" for center ring.
  • Ring O.D. and I.D. are about 3/8" and 3/16", respectively.
  • the outer stainless steel casing 2 supports the rulon column 10 to take the high pressure.
  • the rulon column 10 can be easilymodified to accommodate solid surfaces to study surface charge of coatings.
  • both powders and solid surfaces can be used to determine the ⁇ "-potential of the material of interest. When solid surfaces are used, their distance of separation should be small (10-100 mils) so that adequate pressure drops along the length of the separation can be attained by varying the electrolyte flow.
  • This invention discloses coatings or surfaces to protect measurement surfaces from fouling.
  • the invention makes use of novel techniques to measure both the pH of aqueous solutions and ⁇ "-potentials of substances, coating and surfaces as well as fouling and corrosion products, at high temperatures to discover candidate coatings and surfaces that can be used to prevent fouling.
  • this invention uses measurement of ⁇ "-potentials at elevated temperatures, in the range of about 235°C, to identify candidate coating and surface materials, although measurement at lower and higher temperatures, and under a wide range of pressures and pHs, is also possible using the method of this invention.
  • Deposition of the candidate anti-fouling coatings and anti-fouling surfaces identified herein will be useful when applied to measuring surfaces.
  • a coating which could be applied to a measuring surface, is selected by virtue of its having physicochemical properties which will act to repel particular fouling or corrosion products which are present in a fluid in contactwiththemeasuring surface.
  • the selected coating could then be applied, alone or in a formulation as, for example, by sputtering deposition, electroplating, electrolessplating, ion implantation, and other coating methods known to those skilled in the art, to the measuring surface.
  • Application of the coating to the measuring surface would serve to protect the measuring surface from deposition of all or some of foulingmaterialor corrosionproductspresent in a fluid to be contacted with the measuring surface.
  • a surface which could serve as a measuring surface, is selected by virtue of its having physicochemical properties which will act to repel particular fouling or corroding materials which are present in a fluid in contactwiththemeasuring surface.
  • the selected surface material could be formed as part of or as an addition to the measuring surface, to form a device or the like. Selection of this surfacematerial as the measuring surface would serve to protect the measuring surface from deposition of all or some of foulingmaterial or corrodingmaterial present in a fluid to be contacted with the measuring surface.
  • the feedwater Venturis used to measure mass flow rates in power plants or, for example, orifice plate surfaces or flow tap surfaces or other surfaces susceptible to fouling or corrosion, particularly at high operating temperatures, may be protected.
  • the physicochemical property to bemeasured is the ⁇ "-potential.
  • the ⁇ "-potential of the coating or surface material is compared to the ⁇ "-potential of the fouling material or corroding material, at conditions of temperature and pH that correspond to conditions under which the measuring surface will operate.
  • Such coatings and surfaces will, for example, reduce power losses currently encountered due to venturi fouling and corrosion, and allow more accurate measurements via the measuring surfaces of interest which are critical components in those measurements.
  • the high temperature ⁇ "-potential of oxides as a function of pH has been measured to determine the oxide's pzc's and the sign of the surface charges.
  • ⁇ "-potential measurement is not limitedto oxides, however, andthe ⁇ "-potentials of other fouling and corrosion products, as well as those of a variety of candidate coating and surface materials, are within the scope of this invention.
  • ⁇ "-potentials of various oxides at high temperature have been measured using the above- described apparatus.
  • ⁇ "-potentials are calculated from slopes of the graphs of streaming potential ( ⁇ E) vs. differential pressure ( ⁇ P) .
  • metal oxides having the same sign of surface charge as fouling or corroding material oxides such as Fe 2 0 3 and Fe 3 0 4 , typically found in the feedwater systems of commercial nuclear and fossil fuel power plants, are identified.
  • fouling or corroding material oxides and the candidate metal oxide have the same sign of surface charge at a given pH value, then the candidate metal oxide likely will prevent fouling and/or corrosion of the venturi surface, used to measure mass flow rate of the feedwater entering the system.
  • the pressure in the loop was held at approximately 600 psi; the temperature of the electrolyte in the column was held at 235°C for the course of the measurements. pH of the electrolyte solution was also measured and correlated with the temperature measurements. ⁇ "-potential is calculated from the slope of the graph of streaming potential ( ⁇ E) vs. differential pressure ( ⁇ P). E _ E 0 Dr 2 R ⁇ (7)
  • both PdO and W0 3 show negative ⁇ "-potentials at 235°C over the pH range 2 to 9 and 2 to 6.5, respectively, (Figs. 4 and 5) .
  • BWRs boiling water reactors
  • PWRs pressurized water reactors
  • Fouling and corroding particulates commonly found in venturi ducts of power plants are Fe 2 0 3 and Fe 3 0 4 .
  • characteristics of these compounds were compared to characteristics of PdO and W0 3 .
  • Fe 2 0 3 is negatively charged (Fig. 6) at 235°C and hence, in principle, should not deposit on PdO and W0 3 surfaces due to electrostatic repulsion.
  • Fe 3 0 4 has a small positive charge at 235°C under BWR conditions, indicating some degree of interaction between Fe 3 0 4 and both PdO and W0 3 .
  • Fe 3 0 4 has either a small negative or a small ⁇ _;I ⁇ arge depending on the oxygen content present in the oxide (Fig. 7).
  • Fe 3 0 4 might be slightly attracted or repelled from PdO andW0 3 surfaces. The exact interaction can only be estimated once tests areperformedwith actualpower plant foulingmaterials.
  • the surface charge of the fouling deposits is either close to zero or negative under both BWR and PWR operating conditions (Fig. 8) at 235°C and hence should not deposit on PdO or W0 3 surfaces.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Structural Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Measuring Volume Flow (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

L'invention décrit un procédé de sélection de matériaux de revêtement potentiels pour des applications à haute température. Ce procédé consiste à mesurer les potentiels zêta d'une substance d'encrassement et d'un revêtement ou d'une surface potentiels. La figure représente le dispositif expérimental utilisé pour la mesure du potentiel zêta. La pompe (1) injecte de l'électrolyte dans la boucle (2). Des rubans chauffants (3) sont enroulés autour de la tubulure et sont régulés par des contrôleurs de température (4). Une électrode en YSZ (5) et une électrode de référence (6) à régulation manométrique externe mesurent le pH. La pression du système est mesurée par un manomètre (7) et maintenue par une soupape de décharge (8). La solution est refroidie avec une chemise réfrigérante (9). La substance pulvérulente (11) à mesurer est tassée dans une colonne de rulon (10) et maintenue par des écrans en platine et des filtres en téflon (13). Les contacts d'électrode sont réalisés par l'intermédiaire d'embouts en rulon (14). Un transducteur de pression différentielle (15) est prévu.
PCT/US1992/008238 1991-09-30 1992-09-28 Utilisation et selection de materiaux de revetement et de surface pour lutter contre l'encrassement et la corrosion de surface, par la mesure du potentiel zeta Ceased WO1993007100A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5506989A JPH06504093A (ja) 1991-09-30 1992-09-28 ζ電位測定を用いて表面の汚染及び腐食を制御するための被膜及び表面材料の使用及び選択方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US76918391A 1991-09-30 1991-09-30
US07/769,183 1991-09-30

Publications (1)

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WO1993007100A1 true WO1993007100A1 (fr) 1993-04-15

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EP (1) EP0559879A1 (fr)
JP (1) JPH06504093A (fr)
CA (1) CA2097295A1 (fr)
WO (1) WO1993007100A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4442685C1 (de) * 1994-11-30 1996-03-07 Fraunhofer Ges Forschung Verfahren und Vorrichtung zur Bestimmung eines Strömungspotentials
WO1999050659A3 (fr) * 1998-03-31 2000-01-20 Zetatronics Ltd Procede rapide de detection de micro-organismes et d'evaluation de l'activite antimicrobienne
WO2013041321A1 (fr) * 2011-09-23 2013-03-28 Endress+Hauser Gmbh+Co. Kg Appareil de mesure
EP2816565A4 (fr) * 2012-02-15 2015-11-25 Korea Hydro Nuclear Power Co Ltd Générateur de vapeur de réduction des boues et procédé de fabrication d'une plaque de tube de générateur de vapeur de réduction des boues
CN109781337A (zh) * 2019-01-09 2019-05-21 安徽自动化仪表有限公司 一种用于高温气体管道压力测量的差压变送器

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3764512A (en) * 1972-05-02 1973-10-09 Singer Co Laser scanning electrophoresis instrument and system
US4085021A (en) * 1976-02-02 1978-04-18 Ferro Corporation Electrophoretic porcelain enameling process
US4338363A (en) * 1981-02-17 1982-07-06 The Research Foundation Of State University Of New York Method for inhibiting the formation of scale
US4554176A (en) * 1983-01-31 1985-11-19 Permelec Electrode Ltd. Durable electrode for electrolysis and process for production thereof
US4828790A (en) * 1984-04-20 1989-05-09 Hitachi, Ltd. Inhibition of deposition of radioactive substances on nuclear power plant components
US4970094A (en) * 1983-05-31 1990-11-13 The Dow Chemical Company Preparation and use of electrodes
US5019420A (en) * 1989-01-17 1991-05-28 Eic Laboratories, Inc. Process for forming a reduced electrochromic layer in contact with an ion conducting oxide
US5022972A (en) * 1986-10-28 1991-06-11 MTA Kutatasi Eszkozoket Kivitelezo Vallata Process for measuring and determining zeta-potential in a laminarly flowing medium for practical purposes

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3764512A (en) * 1972-05-02 1973-10-09 Singer Co Laser scanning electrophoresis instrument and system
US4085021A (en) * 1976-02-02 1978-04-18 Ferro Corporation Electrophoretic porcelain enameling process
US4338363A (en) * 1981-02-17 1982-07-06 The Research Foundation Of State University Of New York Method for inhibiting the formation of scale
US4554176A (en) * 1983-01-31 1985-11-19 Permelec Electrode Ltd. Durable electrode for electrolysis and process for production thereof
US4970094A (en) * 1983-05-31 1990-11-13 The Dow Chemical Company Preparation and use of electrodes
US4828790A (en) * 1984-04-20 1989-05-09 Hitachi, Ltd. Inhibition of deposition of radioactive substances on nuclear power plant components
US5022972A (en) * 1986-10-28 1991-06-11 MTA Kutatasi Eszkozoket Kivitelezo Vallata Process for measuring and determining zeta-potential in a laminarly flowing medium for practical purposes
US5019420A (en) * 1989-01-17 1991-05-28 Eic Laboratories, Inc. Process for forming a reduced electrochromic layer in contact with an ion conducting oxide

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4442685C1 (de) * 1994-11-30 1996-03-07 Fraunhofer Ges Forschung Verfahren und Vorrichtung zur Bestimmung eines Strömungspotentials
WO1999050659A3 (fr) * 1998-03-31 2000-01-20 Zetatronics Ltd Procede rapide de detection de micro-organismes et d'evaluation de l'activite antimicrobienne
WO2013041321A1 (fr) * 2011-09-23 2013-03-28 Endress+Hauser Gmbh+Co. Kg Appareil de mesure
EP2816565A4 (fr) * 2012-02-15 2015-11-25 Korea Hydro Nuclear Power Co Ltd Générateur de vapeur de réduction des boues et procédé de fabrication d'une plaque de tube de générateur de vapeur de réduction des boues
CN109781337A (zh) * 2019-01-09 2019-05-21 安徽自动化仪表有限公司 一种用于高温气体管道压力测量的差压变送器

Also Published As

Publication number Publication date
CA2097295A1 (fr) 1993-03-31
EP0559879A1 (fr) 1993-09-15
JPH06504093A (ja) 1994-05-12

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