EP0065877A1 - Industrielles Röntgenstrahlungssystem - Google Patents

Industrielles Röntgenstrahlungssystem Download PDF

Info

Publication number
EP0065877A1
EP0065877A1 EP82302617A EP82302617A EP0065877A1 EP 0065877 A1 EP0065877 A1 EP 0065877A1 EP 82302617 A EP82302617 A EP 82302617A EP 82302617 A EP82302617 A EP 82302617A EP 0065877 A1 EP0065877 A1 EP 0065877A1
Authority
EP
European Patent Office
Prior art keywords
screens
silver halide
industrial
emulsions
gadolinium
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
EP82302617A
Other languages
English (en)
French (fr)
Other versions
EP0065877B1 (de
Inventor
Thomas D. Lyons
Peter B. Jamieson
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.)
3M Co
Original Assignee
Minnesota Mining and Manufacturing Co
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 Minnesota Mining and Manufacturing Co filed Critical Minnesota Mining and Manufacturing Co
Publication of EP0065877A1 publication Critical patent/EP0065877A1/de
Application granted granted Critical
Publication of EP0065877B1 publication Critical patent/EP0065877B1/de
Expired legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C5/00Photographic processes or agents therefor; Regeneration of such processing agents
    • G03C5/16X-ray, infrared, or ultraviolet ray processes

Definitions

  • This invention relates to a novel, high definition, industrial radiographic system.
  • the system uniquely combines fine grain silver halide emulsion photographic film and a light-emitting phosphor screen.
  • Nondestructive testing of articles and materials has become an integral part of quality control in modern manufacturing industries. This type of testing enables on-line and intensive evaluation of the structural soundness of products.
  • One of the most commonly used forms of nondestructive testing is radiographic images taken on industrial materials.
  • Industrial X-rays have been used for many years in the testing of support beams used in the construction of buildings, bridges and the like. They are particularly useful in the evaluation of welds and in testing metal plates for minute flaws which could affect performance.
  • Radiographic emulsions used in industrial screen/film X-ray procedures typically have emulsions where the average grain size is above 0.5 micrometers (e.g., U.S. Patent No. 3,922,545, col. 13, lines 25-46) and generally over 1 micrometer (e.g., U.S. Patent No. 3,753,714, col. 4, lines 34-40).
  • U.S. Patent Nos. 4,177,071 and 4,130,428 discloses a range of 0.25 to 1.2 micrometers for the grain size, but the examples are only of emulsions having average grain sizes of 0.5, 0.6, 0.7 and 0.8 micrometers.
  • An imageable system particularly useful for industrial X-ray procedures comprises at least two X-ray intensifying screens having a radiation sensitive photographic film between the screens.
  • the film comprises a base with a decolorizable (e.g., bleachable or solvent removable in aqueous alkaline solvent) dye underlayer on at least one side of the base and two radiation sensitive silver halide emulsion layers, one on each side of the base (with at least one over the dye underlayer).
  • the silver halide emulsions are comprised of dye sensitized silver halide grains having a number average size of less than 0.40 micrometers and greater than 0.05 micrometers. The grains are preferably sensitized to a portion of the spectral region near that of the light emitted by the; phosphor screen.
  • the present invention concerns itself with radiographic imaging systems comprising two X-ray intensifying screens sandwiching a radiation sensitive element, said element comprising:
  • the present invention also relates to a process for taking industrial radiographic images of industrial materials.
  • 'industrial materials' are defined as all items or artifacts other than life forms.
  • Industrial materials of metals, alloys, ceramics, glass, and polymeric resins (organic and inorganic) in the form of sheets, films, art forms, staple articles, intermediate and completed structures, and other forms are contemplated in the practice of the present invention.
  • Radiographic emulsions used in the practice of the present invention should have silver coating weights less than 10 g Aglin 2 and preferably between 3 and 8 grams of silver per square meter. The most preferred range is between 3 and 7 g/m 2 of silver. These films have enabled complete processing times to be reduced to as little as ninety seconds.
  • the process would be performed by using a conventional X-ray projection source or other high energy particle radiation sources including gamma and neutron sources.
  • the particular phosphor used should have a high absorption coefficient for the radiation emitted from the source.
  • this radiation is high energy particle radiation which is defined as any of X-rays, newtrons and gamma radiation.
  • the industrial material would be placed between the controllable source of X-rays and the industrial radiographic system of the present invention. A controlled exposure of X-rays would be directed from the source and through the industrial material so as to enter and impact the radiographic system at an angle approximately perpendicular to the plane or surface of the intensifying screen and the photographic film contiguous to the inside surface of the screen.
  • the radiation absorbed by the phosphors of the screen would cause light to be emitted by the screen which in turn would generate a latent image in the two silver halide imaging layers.
  • Conventional development processes including stop baths, washes, fixing, bleaching and the like would then be used on the exposed film.
  • the silver halide grains may be selected from amongst any of the known photographic silver halide materials such as silver chloride, silver bromide, silver iodide, silver bromoiodide, silver chlorobromoiodide, silver chlorobromide, and the like and mixtures thereof.
  • photographic adjuvants and processing aids may be used in the practice of the present invention.
  • materials include gelatin extenders, chemical sensitizers (including sulfur and gold compounds), development accelerators (e.g., onium and polyonium compounds), alkylene oxide polymer accelerators, antifoggant compounds, stabilizers (e.g., azaindenes especially the tetra- and pentaazaindenes), surface active agents (particularly fluorinated surfactants), antistatic agents (particularly fluorinated compounds), plasticizers, matting agents, hardening agents, hardening accelerators, and the like.
  • chemical sensitizers including sulfur and gold compounds
  • development accelerators e.g., onium and polyonium compounds
  • alkylene oxide polymer accelerators e.g., antifoggant compounds
  • stabilizers e.g., azaindenes especially the tetra- and pentaazaindenes
  • surface active agents particularly fluorinated surfactants
  • the base may be any one of the well known photographic support materials such as glass, polymeric films such as cellulose acetate (and triacetate), polyesters (particularly polyethyleneterephthalate), polycarbonates, polystyrene, and polyvinyl acetal film base. Many other materials may also be used.
  • photographic support materials such as glass, polymeric films such as cellulose acetate (and triacetate), polyesters (particularly polyethyleneterephthalate), polycarbonates, polystyrene, and polyvinyl acetal film base. Many other materials may also be used.
  • the dye underlayer must contain a decolorizable dye.
  • a decolorizable dye it is meant that the light absorbing ability of the dye must be substantially diminishable or capable of being completely removed.
  • the dye in the binder which forms the underlayer may be readily soluble in aqueous alkaline solutions used in the processing (developing) of the film element so that the dye would be washed out of the element.
  • the dye could be alkaline solution bleachable, heat bleachable, sulfite bleachable, or removable in any other manner which would not require destruction of the image in the film.
  • Heat bleaching of the dyes may be accomplished by selecting dyes which are themselves thermolabile or by combining them with materials which can bleach the dyes when heated.
  • the combination of bleachable dyes with nitrate salts capable of liberating HN0 3 or nitrogen oxides when heated to 160-200°C are particularly desirable.
  • the dye underlayer is particularly important because it prevents cross-talk within the radiographic element.
  • Cross-talk occurs when light emitted from one screen passes through one silver halide emulsion and the base into the second silver halide emulsion and forms a latent image there.
  • the second emulsion i.e., the emulsion on the side of the base away from the emitting screen under consideration
  • the second emulsion is relatively far removed from the screen, the light image is greatly dispersed and the resolution would be greatly reduced. It is, therefore, essential that the dye underlayer absorb radiation of the wavelength emitted by the phosphors.
  • a series of silver halide emulsions with narrow grain size distribution was made in which the grain size was varied from 0.22 to 0.6 micrometers.
  • the emulsions were made using a double jet procedure under controlled pAg conditions.
  • the grains in all cases were iodobromide in composition containing 2.75 mole % iodide and were of cubic habit.
  • the emulsions were handled in the normal manner for coagulating, washing and reconstituting them.
  • the reconstituted emulsions were treated with conventional sulfur and gold sensitizers and were digested at 55°C to increase their sensitivity, cooled to 40°C, and treated with post sensitization additives and stabilizers (namely, tetraazaindines, additional halides, antifoggants, and a spectral sensitizer chosen to provide maximum sensitivity at 550 nm which matches the maximum emission characteristics of 3M's TrimaxO intensifying screen) as is common to the art.
  • post sensitization additives and stabilizers namely, tetraazaindines, additional halides, antifoggants, and a spectral sensitizer chosen to provide maximum sensitivity at 550 nm which matches the maximum emission characteristics of 3M's TrimaxO intensifying screen
  • the photographic films were prepared by separately coating the above emulsion onto both sides of a polyester film base which had previously been coated with an aqueous alkaline soluble dye in a gelatin layer.
  • the film base was 7 mil photograde polyester.
  • the emulsions were applied using a precision photographic coating machine.
  • the final coatings contained 5.1g Ag/m 2 .
  • This example shows the use of the materials of the present invention in commercial industrial radiographic situations.
  • the X-ray intensifying screens used in the practice of the present invention are phosphor screens well known in the art. These phosphors are materials which absorb incident X-rays and emit radiation in a different portion of the electromagnetic spectrum, particularly visible and ultraviolet radiation. Calcium tungstate and rare earth (gadolinium and lanthanum) oxysulfides and gadolinium or lanthanum oxybromides are particularly useful phosphors.
  • the gadolinium oxysulfides and the lanthanum oxysulfides and the phosphates and arsenates can be doped to control the emussion wavelengths and improve their efficiency. Many of these phosphors are shown in U.S. Patent No. 3,725,704 and U.K. Patent No.
  • the phosphate and arsenate phosphors may be generally represented by the formula wherein a is 0.01 to 0.50, b is 0 to 0/50, c is 0 to 0.02, d is o to 0.10, e is 0 to 0.02 and X represents phosphorous or arsenic atoms or mixtures thereof.
  • c is 0, a is 0.05 to 0.30 and d is 0 to 0.02.
  • the sum of b, c, d and e should be greater than zero and should most preferably be at least 0.005.
  • the oxysulfide rare earth phosphors may be represented by the formula wherein Z is the dopant element or elements,
  • g is 0 to 1.99
  • h is 0 to 1.99
  • f is 0.0005 to 0.16.
  • b is 0, a is 0.15 to 1.00, f is 0.0010 to 0.05 and Z is terbium.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Conversion Of X-Rays Into Visible Images (AREA)
EP82302617A 1981-05-26 1982-05-21 Industrielles Röntgenstrahlungssystem Expired EP0065877B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US26740281A 1981-05-26 1981-05-26
US267402 1988-11-04

Publications (2)

Publication Number Publication Date
EP0065877A1 true EP0065877A1 (de) 1982-12-01
EP0065877B1 EP0065877B1 (de) 1986-08-06

Family

ID=23018616

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82302617A Expired EP0065877B1 (de) 1981-05-26 1982-05-21 Industrielles Röntgenstrahlungssystem

Country Status (10)

Country Link
EP (1) EP0065877B1 (de)
JP (1) JPS57198456A (de)
AR (1) AR241831A1 (de)
AU (1) AU550866B2 (de)
BR (1) BR8203024A (de)
CA (1) CA1196733A (de)
DE (1) DE3272443D1 (de)
ES (1) ES8308075A1 (de)
MX (1) MX157370A (de)
ZA (1) ZA823627B (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0245992A2 (de) * 1986-04-29 1987-11-19 E.I. Du Pont De Nemours And Company Aufzeichnungssystem für Radiotherapie
EP0350883A2 (de) * 1988-07-14 1990-01-17 Minnesota Mining And Manufacturing Company Kombination photoempfindlicher Materialien zur Verwendung in der Radiographie
EP0384634A2 (de) * 1989-02-23 1990-08-29 Eastman Kodak Company Radiographische Schirm/Film-Konstruktionen mit verbesserter Quantendetektionsleistungsfähigkeit
EP0437117A1 (de) * 1990-01-10 1991-07-17 Konica Corporation Photographisches lichtempfindliches Silberhalogenidmaterial mit verbesserten diagnostischen Eigenschaften

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1271567A (en) * 1985-05-29 1990-07-10 Cancer Institute Board, (The) Method and apparatus for high engery radiography
AU589980B2 (en) * 1985-05-29 1989-10-26 Cancer Institute Board, The Method and apparatus for high energy radiography
IT1185307B (it) * 1985-07-25 1987-11-12 Minnesota Mining & Mfg Materiali fotosensibili per uso in radiografia e procedimento per la formazione di una immagine radiografica
JP2770205B2 (ja) * 1991-10-24 1998-06-25 富士写真フイルム株式会社 放射線画像読取方法ならびにエネルギーサブトラクション方法

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3005104A (en) * 1958-09-17 1961-10-17 Knapp Mills Inc Method and means for testing metals
US3725704A (en) * 1971-01-28 1973-04-03 Lockheed Aircraft Corp Rare earth phosphors for x-ray conversion screens
US3753714A (en) * 1969-11-21 1973-08-21 Fuji Photo Film Co Ltd Image formation by radiation and intensification
DE2510068A1 (de) * 1974-03-11 1975-09-18 Agfa Gevaert Ag Verbessertes roentgenphotographisches aufnahmematerial
US3922545A (en) * 1974-02-26 1975-11-25 Eastman Kodak Co Process for nondestructively testing with a desensitized silver halide radiographic layer
DE2534105A1 (de) * 1975-01-06 1976-07-08 Dainippon Toryo Kk Verstaerkerschirm fuer die radiographie
DE2540344A1 (de) * 1975-09-10 1977-03-17 Siemens Ag Mit roentgenstrahlen zur fluoreszenz anregbarer leuchtstoff
US4130428A (en) * 1971-11-05 1978-12-19 Agfa-Gevaert, N.V. Combination of photosensitive elements suited for use in radiography
GB1565811A (en) * 1976-06-28 1980-04-23 Minnesota Mining & Mfg Luminescent phosphor materials
US4210715A (en) * 1975-08-02 1980-07-01 Konishiroku Photo Industry Co., Ltd. Light-sensitive silver halide photographic material and method of processing thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5857735B2 (ja) * 1975-01-22 1983-12-21 株式会社日立製作所 放射線検知フイルム
JPS53106125A (en) * 1977-02-28 1978-09-14 Fuji Photo Film Co Ltd Dyestuff image recording
US4259588A (en) * 1979-10-31 1981-03-31 Eastman Kodak Company Green-emitting X-ray intensifying screens

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3005104A (en) * 1958-09-17 1961-10-17 Knapp Mills Inc Method and means for testing metals
US3753714A (en) * 1969-11-21 1973-08-21 Fuji Photo Film Co Ltd Image formation by radiation and intensification
US3725704A (en) * 1971-01-28 1973-04-03 Lockheed Aircraft Corp Rare earth phosphors for x-ray conversion screens
US4130428A (en) * 1971-11-05 1978-12-19 Agfa-Gevaert, N.V. Combination of photosensitive elements suited for use in radiography
US3922545A (en) * 1974-02-26 1975-11-25 Eastman Kodak Co Process for nondestructively testing with a desensitized silver halide radiographic layer
DE2510068A1 (de) * 1974-03-11 1975-09-18 Agfa Gevaert Ag Verbessertes roentgenphotographisches aufnahmematerial
DE2534105A1 (de) * 1975-01-06 1976-07-08 Dainippon Toryo Kk Verstaerkerschirm fuer die radiographie
US4210715A (en) * 1975-08-02 1980-07-01 Konishiroku Photo Industry Co., Ltd. Light-sensitive silver halide photographic material and method of processing thereof
DE2540344A1 (de) * 1975-09-10 1977-03-17 Siemens Ag Mit roentgenstrahlen zur fluoreszenz anregbarer leuchtstoff
GB1565811A (en) * 1976-06-28 1980-04-23 Minnesota Mining & Mfg Luminescent phosphor materials

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0245992A2 (de) * 1986-04-29 1987-11-19 E.I. Du Pont De Nemours And Company Aufzeichnungssystem für Radiotherapie
EP0245992A3 (en) * 1986-04-29 1989-06-28 E.I. Du Pont De Nemours And Company Recording system for irradiation therapy
EP0350883A2 (de) * 1988-07-14 1990-01-17 Minnesota Mining And Manufacturing Company Kombination photoempfindlicher Materialien zur Verwendung in der Radiographie
EP0350883A3 (en) * 1988-07-14 1990-10-31 Minnesota Mining And Manufacturing Company Combination of photosensitive elements for use in radiography
EP0384634A2 (de) * 1989-02-23 1990-08-29 Eastman Kodak Company Radiographische Schirm/Film-Konstruktionen mit verbesserter Quantendetektionsleistungsfähigkeit
EP0384634A3 (de) * 1989-02-23 1990-11-07 Eastman Kodak Company Radiographische Schirm/Film-Konstruktionen mit verbesserter Quantendetektionsleistungsfähigkeit
EP0437117A1 (de) * 1990-01-10 1991-07-17 Konica Corporation Photographisches lichtempfindliches Silberhalogenidmaterial mit verbesserten diagnostischen Eigenschaften

Also Published As

Publication number Publication date
JPS57198456A (en) 1982-12-06
AU550866B2 (en) 1986-04-10
AU8413882A (en) 1982-12-02
EP0065877B1 (de) 1986-08-06
DE3272443D1 (en) 1986-09-11
JPH0473136B2 (de) 1992-11-20
ES512479A0 (es) 1983-08-01
ZA823627B (en) 1983-05-25
MX157370A (es) 1988-11-18
CA1196733A (en) 1985-11-12
ES8308075A1 (es) 1983-08-01
AR241831A1 (es) 1992-12-30
BR8203024A (pt) 1983-05-10

Similar Documents

Publication Publication Date Title
EP0407890B1 (de) Kassette mit Verstärkungsfolie zur Verwendung mit einem Röntgenfilm
US3891852A (en) Neutron detection and radiography
EP0595733B1 (de) Kombination zur Detektion von Weichgewebeanomalien
US5965337A (en) Element for industrial radiography
US4707435A (en) Industrial X-ray system
US4893021A (en) Process for the production of multiple radiographic images
EP0347798A2 (de) Unitarer Verstärkerschirm und radiographisches Element
US4172730A (en) Radiographic silver halide sensitive materials
EP0065877B1 (de) Industrielles Röntgenstrahlungssystem
EP0140666B1 (de) Photothermographisches Aufzeichnungselement für gewerbliche Röntgenphotographie
EP0412730A2 (de) Verbesserte Kassette und Röntgenfilm-Kombination
EP0581065B1 (de) Kombination von lichtempfindlichen Elementen für radiographischen Gebrauch
EP0350883B1 (de) Kombination photoempfindlicher Materialien zur Verwendung in der Radiographie
US20060133561A1 (en) System for industrial radiography
JP4130516B2 (ja) 工業用ラジオグラフィ用製品
JPS6053299B2 (ja) ラジオグラフイ−に有用な感光性要素の組合せ
US6489076B1 (en) Portal imaging assembly with magenta filter and method of use
US6482563B1 (en) Portal imaging assembly with neutral density filter and method of use
US6485880B1 (en) Portal imaging assembly with laminated neutral density filter and method of use
US6489077B1 (en) Portal imaging assembly with pair of asymmetric screens and method of use
EP0939336B1 (de) Neues Erzeugnis und neues Verfahren für industrielle Radiographie
US6485879B1 (en) Portal imaging assembly with asymmetric films and asymmetric screens and method of use
EP1271238A2 (de) Anordnung zur Portalbilderzeugung mit Neutraldichte-Filter und Verfahren zur Verwendung
EP1271239A2 (de) Anordnung zur Portalbilderzeugung mit asymmetrischen Verstärkerschirmen und Verfahren zur Verwendung
Bollen et al. Neutron detection and radiography

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): BE DE FR GB IT NL SE

17P Request for examination filed

Effective date: 19830524

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

ITF It: translation for a ep patent filed

Owner name: BARZANO' E ZANARDO ROMA S.P.A.

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): BE DE FR GB IT NL SE

REF Corresponds to:

Ref document number: 3272443

Country of ref document: DE

Date of ref document: 19860911

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: GB

Ref legal event code: 732

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19900425

Year of fee payment: 9

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19910522

ITTA It: last paid annual fee
EUG Se: european patent has lapsed

Ref document number: 82302617.4

Effective date: 19911209

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19970331

Year of fee payment: 16

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 19970429

Year of fee payment: 16

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19980403

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19980508

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19980529

Year of fee payment: 17

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19980531

BERE Be: lapsed

Owner name: MINNESOTA MINING AND MFG CY

Effective date: 19980531

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19981201

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 19981201

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19990521

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 19990521

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000131

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000301

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST