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EP0205828A1 - Procédé et utilisation d'un acier pour la fabrication de tubes en acier à haute résistance aux gaz acides - Google Patents

Procédé et utilisation d'un acier pour la fabrication de tubes en acier à haute résistance aux gaz acides Download PDF

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Publication number
EP0205828A1
EP0205828A1 EP86105810A EP86105810A EP0205828A1 EP 0205828 A1 EP0205828 A1 EP 0205828A1 EP 86105810 A EP86105810 A EP 86105810A EP 86105810 A EP86105810 A EP 86105810A EP 0205828 A1 EP0205828 A1 EP 0205828A1
Authority
EP
European Patent Office
Prior art keywords
tube
steel
welded
pipe
pipes
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.)
Granted
Application number
EP86105810A
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German (de)
English (en)
Other versions
EP0205828B1 (fr
Inventor
Heinz Dipl.-Ing. Gross
Friedrich-Otto Dipl.-Ing. Koch
Adolf Dr. Peeck
Werner Wennemann
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.)
Hoesch AG
Original Assignee
Hoesch AG
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
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=6272855&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0205828(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Hoesch AG filed Critical Hoesch AG
Priority to AT86105810T priority Critical patent/ATE47428T1/de
Publication of EP0205828A1 publication Critical patent/EP0205828A1/fr
Application granted granted Critical
Publication of EP0205828B1 publication Critical patent/EP0205828B1/fr
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • C21D9/14—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes wear-resistant or pressure-resistant pipes
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/50—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for welded joints

Definitions

  • the invention relates to a method for producing welded steel pipes which can be used for the transport of acidic gases and / or oils, with compressive stresses present on the inside facing the acidic gas and / or oil, and to the use of a steel.
  • H2S hydrogen sulfide
  • acidic The media containing H2S lead to cracks in the pipes, which are referred to as "hydrogen-induced stress corrosion cracking".
  • HIC errors hydrogen-induced cracking
  • SCC errors stress corrosion cracking
  • US Pat. No. 3,992,231 discloses a method for producing oilfield pipes with improved acid gas properties.
  • a steel with 0.28 to 0.42% C, 0.8 to 1.2% Cr, 0.6 to 1.0% Mo, 0.025 to 0.05% Nb, 0.4 up to 1.0% Mn, 0.2 to 0.6% Si, remainder iron and usual unavoidable impurities first of all seamless tubes are produced, which are quenched after an austenitization annealing.
  • the seamless tubes are then placed in an oven at a temperature of 540 ° C to below the transition temperature, i.e. H. Heated to 690 ° C for several hours and then quickly quenched the inner tube wall with water.
  • the tubes produced by this known method are typical oil field tubes with a screw connection, as can be seamlessly manufactured up to a diameter of approximately 500 mm.
  • Large pipes for long-distance lines on the other hand, cannot be seamlessly manufactured due to the process.
  • a steel of the composition mentioned results in poor field weldability, and the long-term heat treatment, for which correspondingly large heating furnaces are required, is technically and economically complex.
  • the intended heat treatment lowers the yield strength of the pipe manufactured, so that higher quality grades can only be obtained by taking appropriate additional measures, such as. B. increased alloy additions of expensive alloy elements can be achieved.
  • DE-OS 34 22 781 Also known from DE-OS 34 22 781 is a method for the heat treatment of an existing pipeline, in which an induction coil placed around the pipeline and a coolant flowing continuously through the pipe are used to generate Build up compressive stresses on the inner surface of the necessary temperature distribution over the wall thickness.
  • the temperature distribution is controlled by a mechanical change in the induction coil geometry (diameter and pitch), which in turn causes a change in the magnetic flux density.
  • the intended continuous internal flow with the cooling medium in the case of single pipe production can only be implemented in a complex manner in terms of plant technology and is characterized by a high demand for cooling medium and high energy input.
  • DE-PS 27 16 081 It is also known from DE-PS 27 16 081 to use a controlled steel with a yield strength of at least 40 HB, consisting of 0.01 to 0.13% carbon, 0.1 to 1.0% silicon, 0.7 to 2.0% manganese, at most 0.1% total aluminum, 0.004 to 0.03% titanium, 0.001 to 0.009% total nitrogen, 0.01 to 0.10% niobium, and 0.01 to 0.15% vanadium and / or 0.05 to 0.40% molybdenum with a total niobium and carbon content of at most 0.005% and at least 0.004% of titanium nitride with a particle size of at most 0.02 ⁇ m, 0 to 0.6% Chromium, 0 to 1.0% copper, 0 to 4.0% nickel on condition
  • HIC heat-affected zone next to the weld seam (Heat Affected Zone).
  • the invention has for its object to provide a method of the type mentioned, by means of which the disadvantages of the methods according to the prior art are avoided and by means of which welded steel pipes with improved resistance to stress corrosion cracking, i. H. in particular, resistance to attack by acidic gases such as hydrogen sulfide, carbonic acid and acidic oils for long-distance pipelines are easy to manufacture and moreover have good field weldability.
  • the invention is based on the object of specifying a method by means of which the above-described errors in the finished, welded tubes for the transport of acidic gases and oils are to be avoided without such a method deteriorating the mechanical properties, in particular the yield strength , d. H. to humiliate.
  • An improvement in the steel structure through globular shaping of the sulfides formed is preferably achieved by adding Ca.
  • Ca instead of or in addition to the calcium, titanium, zirconium and / or rare earths can be added individually or in groups in customary amounts.
  • either the pipe and thus also the weld seam on the outside are continuously section by section using a medium-frequency ring inductor - operated with 0.1 to 5.0 MW - to the required temperature of at least 100 ° C higher than 300 to 300 ° C Heated to 680 ° C and then with a water or air spray plate or only the weld area with the immediately adjacent zone on the outside with the help of a medium frequency line inductor - operated with 0.1 to 5.0 MW - to at least in comparison to the temperature on the inside 100 ° C higher temperature heated from 300 to 680 ° C and then cooled with water or air jets.
  • the welded strip edges or the weld seam can be heated autogenously with gas.
  • this regulation is carried out so that the product of power density in watts per square meter and seam feed speed in meters per second does not fall below a limit value of 10,000 W / (mx sec) with partial internal water or air cooling from 1 to 2,000 liters per meter of pipe length.
  • Essential to the invention is also the use of a steel with a composition according to one or more of claims 1 to 2, which is thermomechanically rolled into a strip, formed into a tube and welded along the longitudinal or spiral seam, internal stresses are built up on the inner surface and a pearlitic-ferritic and / or has a bainitic structure for the transport of acidic gases and / or oils;
  • a steel composed according to claim 6, which is treated according to claim 6, is to be seen as essential to the invention, the compressive residual stresses in the inner surface of the tube being built up to at least one third of the tube wall thickness as tubes for the transport of acidic gases and / or oils .
  • a steel that is treated in the ladle after tapping with a lime-fluorspar slag and flushed with argon and then stripped is further homogenized with calcium in a ladle to produce raw material with the highest degree of purity.
  • the steel is tapped free of slag into the basic pan and rinsed for a few minutes after adding a synthetic slag; after adding lumpy CaSi, the rinsing treatment is continued.
  • the steel has the following melt analysis:
  • the steel is cast into slabs with a dimension of 200 mm thickness and 1,300 mm width in a continuous caster and then the slab reheated to a temperature of 1,170 to 1,250 ° C thermomechanically to a steel strip of 11.9 mm thickness and 1,300 mm width at one Roll temperature of 850 to 910 ° C rolled out.
  • Rolling takes place in three roughing stands, with one pass in the first and third roughing stands and with 3 to 5 passes reversing in the second roughing stand. In the finishing line, rolling is carried out continuously in seven stands.
  • the trimmed steel strip is formed into a spiral pipe with a dimension of 609.6 mm x 11.9 mm (API material X 60) and the adjacent edges of the steel strip are joined together by tack welding and then the pipe is one length from Z. B. 18 m separated.
  • tack-welded pipe is welded through double-sided sub-powder Welding fully welded. Wires and welding powder with a high degree of purity and low hydrogen emission are used for welding.
  • the tubes were heat-treated by means of a device shown in FIG. 2a.
  • Fig. 2a shows a spiral welded tube 1, which rests on guide rollers 2 and is guided by means of further guide rollers 3 on the heat treatment device 4 spirally at a speed of 0.4 m to 30 m per minute.
  • the heat treatment device 4 initially consists of a medium-frequency ring inductor 5, which surrounds the pipe 1 in a width of 50 mm at a distance of 50 mm in a ring and with about 0.1 to 5.0 MW for the ring-shaped heating of the pipe 1 to a temperature is operated from 300 to 680 ° C.
  • a water or air lance 6 is arranged axially, at the head end of which a spray plate 7 is provided at a distance of 5 to 500 mm from the ring inductor 5, by means of which the circumferential zone of the tube 1 heated directly beforehand with the ring inductor 5 sprayed with water or air in a quantity of 1 to 2,000 liters per m pipe and thus cooled.
  • 2aa schematically shows a front view of the medium-frequency ring inductor 5 arranged around the tube 1 and of the spray plate 7 arranged inside the tube 1.
  • a spiral welded tube 1 is also shown, which rests on guide rollers 2 and spirally by means of further guide rollers 3 to another heat treatment device 8, the weld seam 9 is guided past at a speed of 0.4 to 30 m per minute.
  • the heat treatment device 8 consists of a medium-frequency line inductor 10 - operated with 0.1 to 5.0 MW - with a width of 400 mm, past which the weld seam 9 passes and heated to a temperature of 300 to 680 ° C. becomes. Internally.
  • a water or air lance 6 the end of which is bent in a knee shape towards the inner surface of the tube and at the end with a nozzle head 11 in a width which corresponds approximately to the width of the line inductor 10 for spraying water or air in an amount of 1 up to 2,000 liters per m of pipe is provided on the inside of the pipe.
  • 2bb shows a front view of the tube 1 with a line inductor 10 and a bent water or air lance 6 with a nozzle head 11.
  • the tube 1 as shown in FIG. 3 can also be heated autogenously with gas burners 12 to the left and right of the weld seam 13 and then, similar to FIG. 2bb, with a water or air shower 14 are cooled.
  • the arrow 15 indicates the direction of advance of the tube 1.
  • the initial state and the values of the residual stresses inside the pipe obtained by various methods are absolute and related to the yield strength of the treated and tested spiral welded pipes of dimensions 609.6 x 11.9 mm made of material quality X 60 in a bar chart, whereby below this bar chart for the initial state (A) and the methods (B), (D), (E), (H) and (I) schematically the samples with the occurring crack types are assigned. Sections of tubes that were shown or treated as described above were tested. The tube sections were kept in H2S-saturated solution for 96 hours at room temperature. A tensile stress of 44% of the measured yield strength (Rp) of the pipe was applied to the inside of the pipe by ovalizing the pipe section.
  • This initial state is designated by A in FIG. 4, it being evident from the associated sample representation that numerous cracks were found both in the weld seam and in the heat-affected zone.
  • the beam heights, the longitudinal stress and the transverse stress values indicate measured using the disassembly method.
  • the pipes according to D and E were heated to 600 and 700 ° C and then cooled from the outside with water.
  • Q + T quench and temper

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Articles (AREA)
  • Rigid Pipes And Flexible Pipes (AREA)
  • Arc Welding In General (AREA)
  • Heat Treatment Of Steel (AREA)
EP86105810A 1985-06-10 1986-04-26 Procédé et utilisation d'un acier pour la fabrication de tubes en acier à haute résistance aux gaz acides Expired EP0205828B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86105810T ATE47428T1 (de) 1985-06-10 1986-04-26 Verfahren und verwendung eines stahles zur herstellung von stahlrohren mit erhoehter sauergasbestaendigkeit.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3520702 1985-06-10
DE3520702 1985-06-10

Publications (2)

Publication Number Publication Date
EP0205828A1 true EP0205828A1 (fr) 1986-12-30
EP0205828B1 EP0205828B1 (fr) 1989-10-18

Family

ID=6272855

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86105810A Expired EP0205828B1 (fr) 1985-06-10 1986-04-26 Procédé et utilisation d'un acier pour la fabrication de tubes en acier à haute résistance aux gaz acides

Country Status (6)

Country Link
US (1) US4721536A (fr)
EP (1) EP0205828B1 (fr)
JP (1) JPS6254022A (fr)
AT (1) ATE47428T1 (fr)
CA (1) CA1258571A (fr)
DE (1) DE3666461D1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0295500A1 (fr) * 1987-06-03 1988-12-21 Nippon Steel Corporation Tôle d'acier laminée à chaud à haute résistance à la traction et à formabilité excellente
EP0356417A1 (fr) * 1988-08-04 1990-02-28 SCHOELLER-BLECKMANN Gesellschaft m.b.H. Procédé pour la fabrication de pièces tubulaires résistant à la corrosion sous tension, notamment de masses-tiges non magnétisables en acier austénitique et pièces ainsi obtenues
US5181974A (en) * 1990-07-02 1993-01-26 Nippon Steel Corporation Automobile body reinforcing steel pipe
EP0674013A2 (fr) * 1994-03-22 1995-09-27 Nippon Steel Corporation Tôle d'acièr à résistance à la corrosion et à résistance à la fissuration par corrosion sous tension dues aux sulfures
WO1998057085A1 (fr) * 1997-06-13 1998-12-17 Coflexip Procede de fabrication d'une conduite flexible
CN106180981A (zh) * 2016-08-05 2016-12-07 中铁十八局集团第四工程有限公司 超大口径钢管的co2气体保护焊接工艺

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SE8904065L (sv) * 1988-12-07 1990-06-08 Hitachi Ltd Metod att foerbaettra egenskaperna hos svetsare paa austenitiskt rostfritt staal
US5019189A (en) * 1989-04-13 1991-05-28 Kawasaki Steel Corporation Steel pipe and a method for welding thereof and pipeline resistant to carbon dioxide corrosion
JP2503329B2 (ja) * 1991-07-02 1996-06-05 川崎製鉄株式会社 炭酸ガス耐食性および硫化水素ガスに対する耐ｈｉｃ性にすぐれたラインパイプ用鋼
US20030136476A1 (en) * 1997-03-07 2003-07-24 O'hara Randy Hydrogen-induced-cracking resistant and sulphide-stress-cracking resistant steel alloy
US20030116231A1 (en) * 1997-03-07 2003-06-26 O'hara Randy D. Hydrogen-induced-cracking resistant and sulphide-stress-cracking resistant steel alloy
US6149862A (en) * 1999-05-18 2000-11-21 The Atri Group Ltd. Iron-silicon alloy and alloy product, exhibiting improved resistance to hydrogen embrittlement and method of making the same
WO2004097059A1 (fr) * 2003-04-25 2004-11-11 Tubos De Acero De Mexico, S.A. Tube en acier sans jointure susceptible d'etre utilise comme canaliseur et procede d'obtention
US20050076975A1 (en) * 2003-10-10 2005-04-14 Tenaris Connections A.G. Low carbon alloy steel tube having ultra high strength and excellent toughness at low temperature and method of manufacturing the same
DE102004028020A1 (de) * 2004-06-08 2005-12-29 ITT Manufacturing Enterprises, Inc., Wilmington Mehrwandig gerolltes Rohr und Verfahren zu dessen Herstellung
US20060169368A1 (en) * 2004-10-05 2006-08-03 Tenaris Conncections A.G. (A Liechtenstein Corporation) Low carbon alloy steel tube having ultra high strength and excellent toughness at low temperature and method of manufacturing the same
MXPA05008339A (es) * 2005-08-04 2007-02-05 Tenaris Connections Ag Acero de alta resistencia para tubos de acero soldables y sin costura.
JP2009541589A (ja) * 2006-06-29 2009-11-26 テナリス・コネクシヨンズ・アクチエンゲゼルシヤフト 低温における等方じん性が向上した油圧シリンダー用継ぎ目なし精密鋼管およびこれを得る方法
WO2008018980A2 (fr) * 2006-08-04 2008-02-14 Exxonmobil Research And Engineering Company Utilisation de traitement par friction-malaxage et choc laser dans des applications pour pétrole et gaz et pétrochimiques
US20080032152A1 (en) * 2006-08-04 2008-02-07 Vaughn Glen A Use of laser shock processing in oil & gas and petrochemical applications
MX2007004600A (es) * 2007-04-17 2008-12-01 Tubos De Acero De Mexico S A Un tubo sin costura para la aplicación como secciones verticales de work-over.
US7862667B2 (en) 2007-07-06 2011-01-04 Tenaris Connections Limited Steels for sour service environments
WO2009065432A1 (fr) * 2007-11-19 2009-05-28 Tenaris Connections Ag Acier bainitique de haute résistance destiné à des applications octg
US8221562B2 (en) * 2008-11-25 2012-07-17 Maverick Tube, Llc Compact strip or thin slab processing of boron/titanium steels
EP2325435B2 (fr) 2009-11-24 2020-09-30 Tenaris Connections B.V. Joint fileté étanche à des pressions internes et externes [extrêmement hautes]
US9163296B2 (en) 2011-01-25 2015-10-20 Tenaris Coiled Tubes, Llc Coiled tube with varying mechanical properties for superior performance and methods to produce the same by a continuous heat treatment
IT1403688B1 (it) 2011-02-07 2013-10-31 Dalmine Spa Tubi in acciaio con pareti spesse con eccellente durezza a bassa temperatura e resistenza alla corrosione sotto tensione da solfuri.
IT1403689B1 (it) 2011-02-07 2013-10-31 Dalmine Spa Tubi in acciaio ad alta resistenza con eccellente durezza a bassa temperatura e resistenza alla corrosione sotto tensioni da solfuri.
US8636856B2 (en) 2011-02-18 2014-01-28 Siderca S.A.I.C. High strength steel having good toughness
US8414715B2 (en) 2011-02-18 2013-04-09 Siderca S.A.I.C. Method of making ultra high strength steel having good toughness
US9340847B2 (en) 2012-04-10 2016-05-17 Tenaris Connections Limited Methods of manufacturing steel tubes for drilling rods with improved mechanical properties, and rods made by the same
BR112015016765A2 (pt) 2013-01-11 2017-07-11 Tenaris Connections Ltd conexão de tubos de perfuração, tubo de perfuração correspondente e método para montar tubos de perfuração
US9187811B2 (en) 2013-03-11 2015-11-17 Tenaris Connections Limited Low-carbon chromium steel having reduced vanadium and high corrosion resistance, and methods of manufacturing
US9803256B2 (en) 2013-03-14 2017-10-31 Tenaris Coiled Tubes, Llc High performance material for coiled tubing applications and the method of producing the same
EP2789701A1 (fr) 2013-04-08 2014-10-15 DALMINE S.p.A. Tuyaux en acier sans soudure trempé et revenu à paroi moyenne haute résistance et procédé de fabrication des tuyaux d'acier
EP2789700A1 (fr) 2013-04-08 2014-10-15 DALMINE S.p.A. Tuyaux en acier sans soudure trempé et revenu à paroi lourde et procédé de fabrication des tuyaux d'acier
KR102368928B1 (ko) 2013-06-25 2022-03-04 테나리스 커넥션즈 비.브이. 고크롬 내열철강
US20160305192A1 (en) 2015-04-14 2016-10-20 Tenaris Connections Limited Ultra-fine grained steels having corrosion-fatigue resistance
US10295508B2 (en) * 2016-01-06 2019-05-21 Saudi Arabian Oil Company Integrated system for quantitative real-time monitoring of hydrogen-induced cracking in simulated sour environment
RU2629127C1 (ru) * 2016-04-15 2017-08-24 Публичное акционерное общество "Синарский трубный завод" (ПАО "СинТЗ") Способ индукционной термической обработки сварного соединения
US11124852B2 (en) 2016-08-12 2021-09-21 Tenaris Coiled Tubes, Llc Method and system for manufacturing coiled tubing
US10434554B2 (en) 2017-01-17 2019-10-08 Forum Us, Inc. Method of manufacturing a coiled tubing string
CN107511610B (zh) * 2017-08-22 2022-03-25 山东科技大学 一种降低换热器管子和管板焊缝残余应力的设备

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0295500A1 (fr) * 1987-06-03 1988-12-21 Nippon Steel Corporation Tôle d'acier laminée à chaud à haute résistance à la traction et à formabilité excellente
EP0356417A1 (fr) * 1988-08-04 1990-02-28 SCHOELLER-BLECKMANN Gesellschaft m.b.H. Procédé pour la fabrication de pièces tubulaires résistant à la corrosion sous tension, notamment de masses-tiges non magnétisables en acier austénitique et pièces ainsi obtenues
US5181974A (en) * 1990-07-02 1993-01-26 Nippon Steel Corporation Automobile body reinforcing steel pipe
US5192376A (en) * 1990-07-02 1993-03-09 Nippon Steel Corporation Process for producing automobile body reinforcing steel pipe
EP0674013A2 (fr) * 1994-03-22 1995-09-27 Nippon Steel Corporation Tôle d'acièr à résistance à la corrosion et à résistance à la fissuration par corrosion sous tension dues aux sulfures
EP0674013A3 (fr) * 1994-03-22 1996-05-01 Nippon Steel Corp TÔle d'acièr à résistance à la corrosion et à résistance à la fissuration par corrosion sous tension dues aux sulfures.
US5817275A (en) * 1994-03-22 1998-10-06 Nippon Steel Corporation Steel plate having excellent corrosion resistance and sulfide stress cracking resistance
WO1998057085A1 (fr) * 1997-06-13 1998-12-17 Coflexip Procede de fabrication d'une conduite flexible
FR2764669A1 (fr) * 1997-06-13 1998-12-18 Coflexip Procede de fabrication d'une conduite flexible
CN106180981A (zh) * 2016-08-05 2016-12-07 中铁十八局集团第四工程有限公司 超大口径钢管的co2气体保护焊接工艺

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ATE47428T1 (de) 1989-11-15
US4721536A (en) 1988-01-26
JPS6254022A (ja) 1987-03-09
DE3666461D1 (en) 1989-11-23
CA1258571A (fr) 1989-08-22
EP0205828B1 (fr) 1989-10-18

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