EP0447655A1 - Composés photographiques en granulés - Google Patents

Composés photographiques en granulés Download PDF

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Publication number
EP0447655A1
EP0447655A1 EP90124874A EP90124874A EP0447655A1 EP 0447655 A1 EP0447655 A1 EP 0447655A1 EP 90124874 A EP90124874 A EP 90124874A EP 90124874 A EP90124874 A EP 90124874A EP 0447655 A1 EP0447655 A1 EP 0447655A1
Authority
EP
European Patent Office
Prior art keywords
acid
granules
acrylamide
trimethylammonium
methacryloyloxyethyl
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.)
Withdrawn
Application number
EP90124874A
Other languages
German (de)
English (en)
Inventor
Karl-Heinz Reuter
Heinz Dr. Meckl
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.)
Agfa Gevaert AG
Original Assignee
Agfa Gevaert 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
Application filed by Agfa Gevaert AG filed Critical Agfa Gevaert AG
Publication of EP0447655A1 publication Critical patent/EP0447655A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C5/00—Photographic processes or agents therefor; Regeneration of such processing agents
    • G03C5/26—Processes using silver-salt-containing photosensitive materials or agents therefor
    • G03C5/264—Supplying of photographic processing chemicals; Preparation or packaging thereof
    • G03C5/265—Supplying of photographic processing chemicals; Preparation or packaging thereof of powders, granulates, tablets
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C2200/00—Details
    • G03C2200/47—Polymer

Definitions

  • the invention relates to granulated photo chemicals and a process for their production.
  • Photographic processing baths e.g. Developmental, bleaching and fixing baths usually contain the required active ingredients in low concentrations and are therefore prepared by the user himself from water and chemical concentrates as well as, if necessary, other auxiliaries.
  • the concentrates should be dosed as simply as possible and should be largely dust-free. In addition, no unnecessarily high costs should arise for packaging and transport.
  • the liquid concentrates which are generally used in practice for the production of ready-to-use photographic baths have the advantage over the previously used, powdered products that no dust development and no solution problems occur.
  • the concentrates have the disadvantages of the high proportion by weight and volume of water, as well as difficulties in disposing of the bulky packaging.
  • the object of the invention is therefore to find means with which a larger spectrum of photographic processing chemicals can be granulated, the dust content should be further reduced.
  • the granules should also dissolve in water in a short time.
  • the invention therefore relates to photographic processing chemicals in the form of granules with an average particle diameter of 150 to 3000 microns, containing the necessary active ingredients and auxiliary substances, characterized in that the granules additionally contain a polymer having a molecular weight of 500,000 to 14,000,000 in one Amount from 1 to 1000 mg / kg of granules, preferably from 50 to 150 mg / kg of granules, containing at least 80 mol% of acrylamide, acrylic acid, cationic Monomer, or mixtures of acrylamide and cationic or anionic monomer.
  • Suitable cationic comonomers are, for example N-vinylbenzyl-N, N, N-trimethylammonium chloride, N-benzyl-N, N-dimethyl-N-vinylbenzylammonium chloride, N, N, N-trihexyl-N-vinylbenzylammonium chloride, N- (3-maleimidopropyl) -N, N, N-trimethylammonium chloride, N-benzyl-N- (3-maleimidopropyl) -N, N-dimethylammonium chloride, N-vinyloxycarbonylmethyl-N, N, N-trimethylammonium chloride, N- (3-acrylamido-3,3-dimethylpropyl) -N, N, N-trimethylammonium methosulfate, 1,2-dimethyl-5-vinylpyridinium methosulfate, N- (2-hydroxy-3-methacryloyloxypropyl
  • Suitable anionic comonomers are Aconitic acid, 2-acrylamido-2-methylpropanesulfonic acid, 3-acrylamidopropane-1-sulfonic acid, Acrylic acid,
  • Methacrylic acid 4-acryloyloxybutane-1-sulfonic acid, 3-acryloyloxypropionic acid, 3-acryloyloxybutane-1-sulfonic acid, 3-acryloyloxypropane-1-sulfonic acid, 4-t-butyl-9-methyl-8-oxo-7-oxa-4-aza-9-docensulfonic acid, ⁇ -chloroacrylic acid, Maleic acid, Chloromaleic acid, 2-methacryloyloxyethyl-1-sulfonic acid, Citric acid, Crotonic acid, Fumaric acid, Mesaconic acid, ⁇ -methylene glutaric acid, Monoethyl fumarate, Monomethyl- ⁇ -methylene glutarate, Monomethyl fumarate, Vinyl sulfonic acid, p-styrene sulfonic acid, 4-vinylbenzylsulfonic acid, Acryloyloxymethylsulfonic acid, 4-methacryloyloxybut
  • Preferred cationic or anionic comonomers are N-vinylbenzyl-N, N, N-trimethylammonium chloride, N- (3-acrylamido-3,3-dimethylpropyl) -N, N, N-trimethylammonium metho sulfate, N-2- (methacryloyloxyethyl) -N, N, N-trimethylammonium methosulfate, N- (2-methacryloyloxyethyl) -N, N, N-trimethylammonium chloride, 2- (N, N-dimethylamino) ethyl acrylate, N- (2-dimethylaminoethyl) acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, 3-acrylamidopropane-1-sulfonic acid, acrylic acid and methacrylic acid.
  • the remaining monomer components can be (meth) acrylic acid esters, (meth) acrylonitrile, styrene or vinyl esters of acetic or propionic acid.
  • Polyacrylamide, polyacrylic acid and copolymers of acrylamide with the preferred anionic or cationic monomers in any composition are preferred.
  • Suitable photographic processing chemicals are black and white developers, color developers, bleaching agents, fixing agents and bleach-fixing agents.
  • these photographic processing chemicals contain the usual active ingredients and auxiliaries. Details can be found in the exemplary embodiments.
  • the process for producing the granules according to the invention is characterized in that active ingredients and auxiliaries of a photographic processing bath are ground together to a particle size ⁇ 2 mm, preferably 0.5 to 1 mm, then with the addition of a granulating liquid, which contains the copolymer defined above, undergoes powder agglomeration, dries in vacuo and is packaged in a water-vapor-tight manner.
  • the granules produced in this way are mechanically stable, of uniform grain size, show a high dissolution rate and unlimited durability, are dust-free and free-flowing.
  • the solid constituents are usually comminuted to particle sizes of ⁇ 10 ⁇ m by jet milling.
  • the powder agglomeration is preferably carried out in a fluidized bed, the granulation liquid, for example 200 ml of water per kg of powder, being added to the particles to be agglomerated.
  • ком ⁇ онентs of a photographic processing bath can be granulated together, e.g. Antioxidant and alkali dispenser from a color photographic developer, these developer components can be individually granulated, but packed together.
  • a protective gas for example nitrogen.
  • color photographic developer granules contain antioxidants and alkali donors as essential granule components. These three components are preferably granulated separately.
  • the other additives such as anti-limescale, heavy metal complexing agents, sodium sulfite and alkali halide can be granulated together with one or more of the essential components.
  • Suitable color developer compounds are aromatic compounds of the p-phenylenediamine type containing at least one primary amino group, for example N, N-dialkyl-p-phenylenediamines such as N, N-diethyl-p-phenylenediamine, 1- (N-ethyl-N-methanesulfonamidoethyl) -3 -methyl-p-phenylenediamine, 1- (N-ethyl-N-hydroxyethyl) -3-methyl-p-phenylenediamine and 1- (N-ethyl-N-methoxyethyl) -3-methyl-p-phenylenediamine.
  • Other useful color developers are, for example, in. Amer. Chem. Soc. 73 , 3106 (1951) and G. Haist, Modern
  • Bleaching agents contain an iron (III) complex or an iron (III) complex salt and a rehalogenating agent.
  • the bleach granules can contain corrosion inhibitors, for example ammonium nitrate, complexing agents, for example ethylenediaminetetraacetic acid (EDTA), propylenediaminetetraacetic acid (PDTA), diethylenetriaminepentaacetic acid (DTPA) and nitrilotriacetic acid (NTA), and agents for setting the desired pH, for example ammonium carbonate.
  • corrosion inhibitors for example ammonium nitrate
  • complexing agents for example ethylenediaminetetraacetic acid (EDTA), propylenediaminetetraacetic acid (PDTA), diethylenetriaminepentaacetic acid (DTPA) and nitrilotriacetic acid (NTA)
  • EDTA ethylenediaminetetraacetic acid
  • PDTA propylenediaminetetraacetic acid
  • DTPA diethylenetriaminepentaacetic acid
  • NTA nitrilotriacetic acid
  • the Fe (III) complexes or complex salts are the Fe (III) complexes or (NH4) Fe (III) complex salts of EDTA, PDTA, DTPA and NTA.
  • Suitable rehalogenating agents are alkali and ammonium halides, e.g. NaBr, KBr, NH4Br and NaCl.
  • the iron (III) complex or the iron (III) complex salt preferably makes up 20 to 50% by weight of the finished granules; the rehabilitation agent preferably makes up 40 to 70% by weight of the finished granulate.
  • Fixatives usually contain a thiosulfate, e.g. Ammonium or sodium thiosulfate.
  • thiosulfate e.g. Ammonium or sodium thiosulfate.
  • Complexing agents such as ethylenediaminetetraacetic acid and agents for adjusting the desired pH such as sodium carbonate can be considered as further constituents of the fixing agents.
  • the bleaching agent and fixing agent are granulated together. In this case, the addition of a rehalogen is not necessary.
  • the mixture is comminuted in an Alexander mill to about 0.5-0.6 mm grain size and granulated in an air stream on a commercially available fluidized bed granulator (Strea 1 laboratory device from Aeromatic, Bubendorf / Switzerland).
  • drying is carried out in the same device by heating the fluidizing air to 60 ° C. for 4-5 minutes.
  • the granulate is free-flowing, but very dusty. If you screen off the dust content, new dust particles quickly form again, caused by strong abrasion.
  • Polyacrylamide A is a polyacrylamide with an average molecular weight of 7 ⁇ 106 ⁇
  • a bleach-fix bath granulate is produced by mixing two individual granules A and B. The following quantities of chemicals are used for 10 l ready-to-use regenerator:
  • the chemicals listed under A are ground in an Alexander mill to about 1 mm grain size and then ground in an air jet mill to a particle size of 5 microns.
  • the ground material is then granulated in about 500 g portions on the fluidized bed granulator mentioned in Example 1.
  • 50 ml of water as granulating liquid are sprayed into the fluidized bed within about 2 minutes.
  • the mixture is then dried by heating the fluidizing air to 70 ° C. for about 6 minutes.
  • the gut grain is separated from about 5% undersize ( ⁇ 0.2 mm) by sieving. It is then dried in vacuo at room temperature.
  • the chemicals listed under B are granulated in about 7 minutes by spraying on 50% by weight ammonium iron EDTA solution which contains excess ammonia. 200 ml of this solution are sprayed onto 600 g of mixture B at room temperature. The mixture is then dried by heating the fluidizing air to 70 ° C. for 10 minutes. After the oversize has been sieved, it is dried for 3 to 4 hours in vacuo at room temperature.
  • Granules A and B are mixed to produce the ready-to-use mixed granulate.
  • 911 g of granules A and 578 g of granules B provide the required amount of mixed granules for 10 l of bleach-fixer regenerator.
  • This ground material is then granulated in 500 g portions on the commercially available Strea-1 fluidized bed granulator.
  • 60 ml of the 0.05% strength by weight aqueous solution of a 1: 1 copolymer of acrylamide and acrylic acid with an average molecular weight of 11.10masse are sprayed on as the granulating liquid in about 5 minutes.
  • drying is carried out by heating the fluidizing air to 70 ° C. for 6 minutes.
  • the granules obtained are then dried in vacuo at room temperature for 3 hours after sieving about 1% by weight oversize.
  • Example 4 The result is a dust-free, free-flowing and quickly soluble granulate. Compared to Example 3, the one-step process of Example 4 is much simpler.
  • the mixture After comminution on the Alexander mill, the mixture is ground in an air jet mill to an average particle size of about 5 ⁇ m.
  • Example 1 About 700 g of this mixture are per batch in the granulator used in Example 1 by spraying 110 ml of water granulated within 5 min. The spraying is interrupted several times in order to achieve an even grain size distribution. The granules obtained are then dried by heating the fluidizing air to 55 ° C. for 10 minutes. Any oversize or undersize is screened off. This is followed by drying in vacuo at room temperature for 2 hours.
  • the granules are slightly dusty and tend to stick together.
  • a dust-free, free-flowing granulate is obtained which does not tend to cake.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Detergent Compositions (AREA)
EP90124874A 1990-03-23 1990-12-20 Composés photographiques en granulés Withdrawn EP0447655A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4009310A DE4009310A1 (de) 1990-03-23 1990-03-23 Granulierte fotochemikalien
DE4009310 1990-03-23

Publications (1)

Publication Number Publication Date
EP0447655A1 true EP0447655A1 (fr) 1991-09-25

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ID=6402867

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90124874A Withdrawn EP0447655A1 (fr) 1990-03-23 1990-12-20 Composés photographiques en granulés

Country Status (4)

Country Link
US (1) US5135840A (fr)
EP (1) EP0447655A1 (fr)
JP (1) JPH04221951A (fr)
DE (1) DE4009310A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0540296A1 (fr) * 1991-10-28 1993-05-05 Konica Corporation Agent de traitement pour la photographie
EP0542283A1 (fr) * 1991-11-12 1993-05-19 Konica Corporation Comprimé pour la traitement d'un matériau photographique à l'halogénure d'argent sensible à la lumière
EP0547796A1 (fr) * 1991-12-17 1993-06-23 Konica Corporation Composés chimique sous forme solide utilisé dans la traitement d'un matériau photographique à l'halogénure d'argent sensible à la lumière
EP0580372A2 (fr) * 1992-07-16 1994-01-26 Konica Corporation Composé pour traitement photographique, noir et blanc
EP0638843A2 (fr) * 1993-07-29 1995-02-15 Konica Corporation Agent solide de traitement pour matériau photographique à l'halogénure d'argent sensible à la lumière
EP0683430A2 (fr) * 1994-05-17 1995-11-22 Polaroid Corporation Compositions de traitement photographiques incluant un agent éprassissant hydrophobiquement modifié

Families Citing this family (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2687043B2 (ja) * 1990-04-27 1997-12-08 富士写真フイルム株式会社 ハロゲン化銀カラー写真感光材料の処理方法
US6096488A (en) * 1990-04-27 2000-08-01 Fuji Photo Film Co., Ltd. Method for processing silver halide color photographic material
US5240822A (en) * 1990-07-30 1993-08-31 Konica Corporation Packed photographic solid processing agents
DE4025560A1 (de) * 1990-08-11 1992-02-13 Agfa Gevaert Ag Fotochemikalien mit vermindertem staubanteil
US5780211A (en) * 1991-05-01 1998-07-14 Konica Corporation Processing composition in the tablet form for silver halide photographic light-sensitive material
DE4120867A1 (de) * 1991-06-25 1993-01-07 Agfa Gevaert Ag Fotografisches verarbeitungsverfahren und vorrichtung dafuer
US5278036A (en) * 1991-09-24 1994-01-11 Konica Corporation Photographic developer composition
JP2843877B2 (ja) * 1992-01-18 1999-01-06 コニカ株式会社 写真用処理剤
US5270154A (en) * 1992-01-31 1993-12-14 Fuji Hunt Photographic Chemicals Inc. Method of making flowable alkaline thiosulfate/alkaline sulfite and the product thereof
JP3084119B2 (ja) * 1992-02-25 2000-09-04 コニカ株式会社 ハロゲン化銀写真感光材料の処理方法
JPH0627619A (ja) * 1992-05-13 1994-02-04 Fuji Photo Film Co Ltd カラー写真用漂白定着組成物
US5384233A (en) * 1992-06-15 1995-01-24 Konica Corporation Chemicals kit including a container formed of multilayer film, for processing photographic light-sensitive materials
JPH0643604A (ja) * 1992-07-25 1994-02-18 Konica Corp ハロゲン化銀写真感光材料の処理方法
US5480768A (en) * 1993-02-17 1996-01-02 Konica Corporation Method for processing exposed silver halide photographic light-sensitive material using a solid processing composition replenisher
JPH07114151A (ja) * 1993-08-23 1995-05-02 Konica Corp ハロゲン化銀写真感光材料用固体処理剤
DE69520079T2 (de) 1994-04-19 2001-06-21 Konishiroku Photo Ind Herstellungsverfahren für feste Verarbeitungszusammensetzungen für photographische, lichtempfindliche Silberhalogenidmaterialien
JPH0829924A (ja) * 1994-05-09 1996-02-02 Konica Corp ハロゲン化銀カラー写真感光材料用発色現像剤造粒物、その造粒方法、該造粒物を用いた固体処理剤および錠剤型固体処理剤
CA2195959A1 (fr) * 1994-08-19 1996-02-29 Neil A. Randen Adhesifs a base d'eau
US5624793A (en) * 1994-11-11 1997-04-29 Konica Corporation Method of manufacturing solid processing composition for silver halide photographic light-sensitive materials
US5618658A (en) * 1995-02-22 1997-04-08 Fuji Hunt Photographic Chemicals, Inc. Process for producing an ammonium thiosulfate product
JPH0990573A (ja) * 1995-09-28 1997-04-04 Konica Corp ハロゲン化銀写真感光材料の処理用固体現像補充剤及び現像処理方法
JP3508081B2 (ja) * 1995-10-30 2004-03-22 コニカミノルタホールディングス株式会社 ハロゲン化銀写真感光材料用固体処理剤および処理方法
JP3663858B2 (ja) * 1997-11-05 2005-06-22 コニカミノルタホールディングス株式会社 ハロゲン化銀写真用固体処理剤及びその製造方法
US5922521A (en) * 1998-03-26 1999-07-13 Eastman Kodak Company Uniformly mixed dry photographic processing composition and method of preparation
US5945265A (en) * 1998-03-26 1999-08-31 Eastman Kodak Company Uniformly mixed dry photographic developing composition containing antioxidant and method of preparation
JP2004264678A (ja) * 2003-03-03 2004-09-24 Fuji Photo Film Co Ltd 顆粒型写真用固体処理剤及びその製造方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1272710A (en) * 1969-09-11 1972-05-03 Ver Kunstmestf Mekog Albatros Process for the granulating of powdery substances
GB1310695A (en) * 1969-08-06 1973-03-21 Ebara Infilco Granulating method
GB1325694A (en) * 1969-08-29 1973-08-08 Kao Corp Method of forming granular products
US3981372A (en) * 1975-03-31 1976-09-21 Lorenzo Moreau Motorized snow vehicle stand
GB1474112A (en) * 1973-03-16 1977-05-18 Ciba Geigy Ag Process for the preparation of non-dusty easily wetted and readily soluble granulates
GB2112954A (en) * 1981-12-24 1983-07-27 Konishiroku Photo Ind Developer composition
EP0358034A2 (fr) * 1988-09-03 1990-03-14 Agfa-Gevaert AG Développateur granulé pour la photographie en couleur et sa préparation

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2543086A (en) * 1947-11-22 1951-02-27 Eastman Kodak Co Method of preparing dustless photographic fixing powders
GB647409A (en) * 1948-01-07 1950-12-13 Eastman Kodak Co Improvements in and relating to photographic fixing powders
US2759823A (en) * 1954-07-26 1956-08-21 Eastman Kodak Co Preparation of fixing powders

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1310695A (en) * 1969-08-06 1973-03-21 Ebara Infilco Granulating method
GB1325694A (en) * 1969-08-29 1973-08-08 Kao Corp Method of forming granular products
GB1272710A (en) * 1969-09-11 1972-05-03 Ver Kunstmestf Mekog Albatros Process for the granulating of powdery substances
GB1474112A (en) * 1973-03-16 1977-05-18 Ciba Geigy Ag Process for the preparation of non-dusty easily wetted and readily soluble granulates
US3981372A (en) * 1975-03-31 1976-09-21 Lorenzo Moreau Motorized snow vehicle stand
GB2112954A (en) * 1981-12-24 1983-07-27 Konishiroku Photo Ind Developer composition
EP0358034A2 (fr) * 1988-09-03 1990-03-14 Agfa-Gevaert AG Développateur granulé pour la photographie en couleur et sa préparation

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0540296A1 (fr) * 1991-10-28 1993-05-05 Konica Corporation Agent de traitement pour la photographie
US5362610A (en) * 1991-10-28 1994-11-08 Konica Corporation Photographic processing agent
EP0542283A1 (fr) * 1991-11-12 1993-05-19 Konica Corporation Comprimé pour la traitement d'un matériau photographique à l'halogénure d'argent sensible à la lumière
EP0547796A1 (fr) * 1991-12-17 1993-06-23 Konica Corporation Composés chimique sous forme solide utilisé dans la traitement d'un matériau photographique à l'halogénure d'argent sensible à la lumière
EP0580372A2 (fr) * 1992-07-16 1994-01-26 Konica Corporation Composé pour traitement photographique, noir et blanc
EP0580372A3 (en) * 1992-07-16 1995-08-23 Konishiroku Photo Ind Black-and-white photographic processing compound
EP0638843A2 (fr) * 1993-07-29 1995-02-15 Konica Corporation Agent solide de traitement pour matériau photographique à l'halogénure d'argent sensible à la lumière
EP0638843A3 (fr) * 1993-07-29 1996-03-06 Konishiroku Photo Ind Agent solide de traitement pour matériau photographique à l'halogénure d'argent sensible à la lumière.
EP0683430A2 (fr) * 1994-05-17 1995-11-22 Polaroid Corporation Compositions de traitement photographiques incluant un agent éprassissant hydrophobiquement modifié
EP0683430A3 (fr) * 1994-05-17 1996-12-27 Polaroid Corp Compositions de traitement photographiques incluant un agent éprassissant hydrophobiquement modifié.

Also Published As

Publication number Publication date
DE4009310A1 (de) 1991-09-26
US5135840A (en) 1992-08-04
JPH04221951A (ja) 1992-08-12

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