US3392019A - Viscous silver halide photographid monobath solutions - Google Patents

Viscous silver halide photographid monobath solutions Download PDF

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Publication number
US3392019A
US3392019A US590473A US59047366A US3392019A US 3392019 A US3392019 A US 3392019A US 590473 A US590473 A US 590473A US 59047366 A US59047366 A US 59047366A US 3392019 A US3392019 A US 3392019A
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United States
Prior art keywords
monobath
silver
amine
silver halide
photographic
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Expired - Lifetime
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US590473A
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English (en)
Inventor
John C Barnes
Gerald J Johnston
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Eastman Kodak Co
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Eastman Kodak Co
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Publication date
Priority to FR969478A priority Critical patent/FR1394373A/fr
Priority to BE646136A priority patent/BE646136A/xx
Priority to DE19641447637 priority patent/DE1447637A1/de
Priority to GB14460/64A priority patent/GB1066993A/en
Application filed by Eastman Kodak Co filed Critical Eastman Kodak Co
Priority to US590473A priority patent/US3392019A/en
Application granted granted Critical
Publication of US3392019A publication Critical patent/US3392019A/en
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    • 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
    • G03C5/58—Processes for obtaining metallic images by vapour deposition or physical development
    • 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
    • G03C5/38—Fixing; Developing-fixing; Hardening-fixing
    • G03C5/383—Developing-fixing, i.e. mono-baths
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S430/00—Radiation imagery chemistry: process, composition, or product thereof
    • Y10S430/135—Cine film

Definitions

  • This invention relates to photography and more particularly to viscous monobaths used for developing and stabilizing photographic silver halide emulsions.
  • Monobaths for processing photographic emulsions in a single bath have been proposed which would contain both the developing agent and the stabilizing or fixing agent in a single bath so that the photographic emulsion would be both developed and stabilized at the same time.
  • a single processing solution of the monobath type be prepared in a viscous condition so that it could be applied to the surface of a photographic emulsion in a rapid processing operation.
  • Monobaths are particularly useful in connection with Reader-Printers for microfilm in which the photographic light-sensitive paper is stored in the printer in roll form and copies are made from microfilm by exposing the sensitized paper to the desired subject matter and processin in a monobath.
  • the monobath for a Reader-Printer should preferably be adequate to provide 20 prints per day for working days without exhaustion.
  • the bath must withstand exposure to air during that time and must hold its complexed silver to prevent the formation of sludge or silver plating on the processor.
  • the bath must provide satisfactory quality prints throughout the life of the bath and should withstand more than four weeks storage at 120 F. in a closed container.
  • the bath should be stable at reduced temperature conditions so that it will remain in solution after at least 24 hours in a closed container at about 34 F.
  • clearing of the print must be relatively fast to provide copies in a short time.
  • the simple incorporation of the fixing compound, a water-soluble thiosulfate, in a developer solution containing a typical silver halide developer such as hydroquinone has an eifect on the photographic emulsion of decreasing the constrast and density and also producing undesirable silver sludge in the monobath,
  • a typical silver halide developer such as hydroquinone
  • many other components have been proposed for use in monobaths along with components which increase the clearing rate of the photographic emulsion and result in low fog levels.
  • the addition of development nuclei results in low fog levels and rapid clearing, but these nucleated particles tend to adhere to the surface of the emulsion.
  • Amines have been suggested for use in monobaths, in order to provide increased speed and contrast. However, many amines cannot be used since they cause a loss in speed and contrast or excessive fog levels.
  • One of the objects of this invention is to provide a viscous monobath containing a combination of at least one amine compound, physical development nuclei and a thickening agent. Another object is to provide a monobath having reduced processing time and an improved speedfog relationship. An additional object is to provide a monobath which results in reduced granularity in the silver halide emulsion and which has increased temperature latitude. A further object is to provide a monobath having minimized sensitivity to the accumulation of bromide and iodide ions resulting from processing reactions which will permit rejuvenation of the monobath. Another object is to provide a monobath having increased contrast and improved processing uniformity over previously known monobaths. Another object is to provide a method of processing exposed photographic elements employing a novel monobath. Additional objects will become apparent hereinafter.
  • a monobath which comprises an aqueous alkaline solution containing a photographic de veloping agent .for reducing exposed silver halide to metallic silver and a water-soluble thiosulfate fixing agent in sufiicient quantity to stabilize substantially all unexposed silver halide.
  • the physical development nuclei are present in a concentration of from about 0.05 to about 2.0 grams per liter of monobath solution and can be any material suitable for this purpose and includes, for example, colloidal silver or the colloidal sulfides and selenides of the metals of group Ib, IIb, Nb and VIII of the Periodic Table including zinc, cadmium, nickel, silver, etc.
  • the particle size is not particularly important to the operation of our monobath, the particles preferably have an average diameter of 72,500 A.
  • the thickening agent can be any material suitable for giving a desired viscosity to the monobath and includes, for example, a water-soluble polymer or gum such as guar gums, nonhydrolyzable cellulose esters such as carboxymethylcellulose or hydroxyethylcellulose, silica gel, starch, etc.
  • Sufiicient thickening agent is used to produce a viscosity of at least about 50 cps., but not more than about 20,000 cps. at 24 C.
  • the guar gums which can be used in this invention are mainly galactomannan. This material is a high molecular weight, carbohydrate polymer or polysaccharide made up of many mannose and galactose units linked together. In actual practice, the commercial product is obtained from guar and contains smaller quantities of protein, crude fiber and inorganic material.
  • guar gum used herein and in the appended claims refers to the above compounds obtained from guar which may have a galactomannan content of from 50 to over 95 percent.
  • the amine compound can be either morpholine, a hydroxyalkyl amine containing a single hydroxyl group and wherein the hydroxyalkyl group has 1-5 carbon atoms, a sulfur dioxide addition product of morpholine or a sulfur dioxide addition product of said hydroxyalkyl amine.
  • Another way of defining the hydroxyalkyl amine is the following general formula:
  • R represents a hydroxyalkyl group having 1 to carbon atoms and R and R each represent a hydrogen atom or an alkyl hydrocarbon group having 1 to 3 carbon atoms.
  • Typical amine compounds which can be used in the invention are, for example, Z-aminoethanol, 2- methylaminoethanol, 2-ethylaminoethanol, Z-dimethylaminoethanol, Z-diethylaminoethanol, or morpholine.
  • a mixture of the amine and the sulfur dioxide addition product of the amine has also been found to give very good results. About /2-2 equivalents of amine per liter of monobath solution is a preferred concentration.
  • any of the known black-and-white photographic developing agents can be used in the monobath of the invention. These developing agents can be employed alone or in combination such as, for example, a 3-pyrazolidone in combination with hydroquinone, N-methyl-p-aminophenol sulfate, chlorohydroquinone, etc.
  • concentration of the developing agent in the monobath composition can be varied, depending upon the particular photographic material undergoing development.
  • Another embodiment of the invention is to incorporate the photographic developing agents mentioned above into the photographic element itself so that the processing solution would then only contain a fixing agent, physical development nuclei, a thickening agent and the amine compound.
  • the developing agent may be incorporated directly into the emulsion layer or in a layer contiguous to the emulsion layer.
  • the 3-pyrazolid0ne developing agents were found to be particularly useful for this application as were development precursors such as 3-acetoxy-1-phenyl-3-pyrazolidone.
  • hydroquinone with an auxiliary developing agent as set forth in the examples illustrates our preferred embodiment. It is desirable to use an auxiliary developer which increases the speed of the develop ing action. Any of the known auxiliary developers which increase the speed of hydroquinone as a developing agent may be used.
  • Typical auxiliary developing agents include those described in application Ser. No. 134,014, filed Aug. 25, 1961, of P. H. Stewart, G. E. Fallesen and I. W. Reeves, Jr., now abandoned.
  • Auxiliary agents described in this application include 3-pyrazolidone compounds containing any alkyl (e.g., methyl, ethyl, etc.) or aryl substituent (e.g., phenyl, p-tolyl, etc.).
  • such prazolidone developing agents can contain an acyl or acyloxy substituent which can be hydrolyzed from the 3-pyraz0lidone compound by treatment with an alkaline activator solution to produce the desired auxiliary developing compound.
  • Typical auxiliary developing agents include, for example, 1 phenyl 3 pyrazolidone, 1 p tolyl-3-pyrazolidone, 1 phenyl 5 methyl 3 pyrazolidone, 1- acetamidophenyl-3-pyrazolidone, 3 acetoxyl-l-phenyl-3- pyrazolidone (enol ester), Z-(pyridinium acety1)-1- phenyl-3-pyrazolidone chloride, 1-phenyl-4,4-dirnethyl-3- pyrazolidone, l phenyl 2- laur0yl-3-pyrazolidone, lphenyl-Z-chloroacetyl-3-pyrazolidone, etc.
  • auxiliary developing agents can be varied and, of course, no auxiliary developing agent need be employed unless so desired.
  • Useful concentrations of auxiliary developing agents vary from about 0.005 mol to 0.5 mol per mol of developing agent. Depending upon the particular auxiliary developing agent employed, larger or smaller quantities can be used.
  • certain other developing agents can be used with the hydroquinone compounds of our invention provided theyhave the same speed as the combination of hydroquinone with an auxiliary developing agent of the type described above.
  • the amount of silver halide developing agent can be varied widely depending upon the agent used and the particular silver halide emulsion. However, a preferred range is about between 1 to 20 grams per liter. It will also be appreciated that while in some instances a halide salt such as potassium iodide, potassium bromide, or the like is desirable, this is not a necessary component of the monobath. A water-soluble sulfite is desirable in the monobath in an amount at least sutficient to prevent preliminary oxidation of the developing agents, but may be omitted where the sulfur dioxide addition product of the amine is used.
  • the water-soluble thiosulfate fixing agent used in the monobath can be any of these suitable for the intended purpose and can be used in any quantity suificient to fix or stabilize substantially all of the unexposed silver halide.
  • Suitable compounds include sodium thiosulfate, potassium thiosulfate, ammonium thiosulfate, etc.
  • a particularly useful concentration for the thiosulfate compound was found to be at least about 20 grams per liter.
  • the maximum concentration of the thiosulfate compound is primarily a function of the concentration of the silver halide in the emulsion being processed.
  • concentra tions as high as 200 grams of thiosulfate per liter of monobath composition can be employed and good quality images can be produced in 5 seconds or less usin such compositions.
  • concentration of silver halide in the emulsion is increased, then it is possible that amounts of thiosulfate in excess of 200 grams per liter can be employed.
  • the pH of the monobath compositions of our invention can be varied, but especially useful results have been obtained at pHs of at least about 9.5 to pHs as high as about 12 or 12.5.
  • the silver halide emulsion of the photographic elements which can be processed in accordance with this invention may be sensitized using any of the well-known techniques in emulsion making, for example, 'by digesting with naturally active gelatin or various sulfur, selenium, tellurium compounds and/ or gold compounds.
  • the emulsions can be sensitized with salts of noble metals of Group VIII of the Periodic Table which have an atomic weight greater than 100.
  • the emulsions may also contain speed increasing addenda such as quaternary ammonium salts, polyethylene glycols or 'thioethe-r sensitizers.
  • the silver halide emulsion of the photographic elements which can be processed according to this invention may also contain conventional addenda such as gelatin plasticizers, coating aids, and hardeners such as alkali metal bisulfite-aldehyde addition products such as sodium formaldehyde 'bisulfi-te, glutaraldehyde bis(sodium bisulfite), beta-methyl glutaraldehyde bis(sodium bisulfite), maleic dialdehyde bis(sodium bisulfite) and the like.
  • These emulsions may be useful in X-ray and other nonoptically sensitized emulsions, and may also be used in orthochromatic, panchromatic, and infrared sensitive emulsions.
  • the addenda may be added to the emulsion before or after sensitizing dyes, if any are used. Sensitizing dyes useful in sensitizing such emulsions are decribed, for
  • Spectral sensitizers which can be used are the cyanines, merocyanines, complex (trinuclear) cyanines, complex (trinuclear) merocyanines, styryls and hemicyanines.
  • Various silver salts may be used as the sensitive salt such a silver bromide, silver iodide, silver chloride, or mixed silver halides such as silver chlorobromide or silver bromoiodide.
  • the silver halides used can be those which form latent images predominantly on the surface of the silver halide grains or those which form latent images inside the silver halide crystals as exemplified by Davey and Knott US. Patent 2,592,250 as Well as direct positive emulsions such as those described in Kendall and Hill US. Patent 2,541,-
  • the silver halide emulsion layer of the photographic elements which can be processed according to the instant invention can contain any or the hydrophilic water-permeable binding materials suitable for this purpose. Suitable materials include gelatin, colloidal albumin, polyvinyl compounds, cellulose derivatives, acrylamide polymers, etc. Mixtures of these binding agents can also be used.
  • the binding agents for the emulsion layer of the photographic element can also contain dispersed polymerized vinyl compounds. Such compounds are disclosed, for example, in US.
  • the silver halide emulsion of the photographic elements which can be processed according to the instant invention may be coated on a wide variety of supports.
  • Typical supports are cellulose nitrate film, cellulose ester film, polyvinyl acetal film, polystyrene film, poly(ethylene terephthalate) film and related films or resinous materials as well as glass, paper, metal and the like.
  • Supports such as paper which are coated with a-olefin polymers, particularly polymers of a-olefins containing two or more carbon atoms, as exemplified by polyethylene, polypropylene, ethylene-butene c-opolymers and the like can also be employed.
  • Example 1 Methyl'aminoethanol-sulfur dioxide addition product (17.8% S grams 75.0 1-phenyl-4,4-dimethyl-3 pyrazolidone do 2.0 Hydroquinone do- 10.0 Sodium thiosulfate crystal do 50.0 Potassium iodide do 0.5 P 10.5 Water to make 1.0 liter. Colloidal silver (Carey Lea Silver) "gram” 0.2 Natrosol (hydroxyethylcellulose) do 0.2
  • This monobath was appliedto the surface of an exposed silver bromoiodide emulsion, and after standing for minutes at70 F. was washed away to exhibit a very high quality, completely developed and fixed image. Photographic properties such as speed, contrast, granularity, and acutance are equal to those produced when this film is developed in the normal way using D-76 followed by separate fixation.
  • Example 4 The above Examples 1, 2 and 3 were repeated substituting zinc sulfide, nickel sulfide, lead sulfide, silver sulfide, and copper sulfide as the nuclei in place of the colloidal silver.
  • the monobaths provided the same high degree of photographic processing as were obtained using the colloidal silver.
  • a silver bromoiodide emulsion was processed in each of the 18 monobaths for various times ranging from 1 to 16 minutes (with no agitation). This was accomplished in three dilferent ways:
  • the 2 -aminoethanol monobath exhibited a much higher clearing rate and a much higher development rate than did the sodium carbonate monobath. In this case, and in all subsequent cases, except with tetramethylammonium bromide, the concentration of the alkaline ingredients are nearly equivalent.
  • the four amines in Group I increased both development rates and clearing rates, but appeared to proportionately increase development rate more than clearing rate.
  • the two amines in Group II also increased both development and clearing rates, but did not increase the development rate significantly.
  • the amine in Group III as was also the case with sodium hydroxide, increased clearing rate and did not increase development rate.
  • the pattern of behavior is not dependent upon the type of amine, i.e., whether primary, secondary, or tertiary, since samples of all three types are found in Group I.
  • the amines in Group I produced increases in density, while amines in Groups II and III produced decreases in density.
  • This invention is thus concerned exclusively with amines of Group I.
  • This monobath was used to process a low speed finegrain chlorobromide emulsion at F. After 15 seconds, the film is completely developed and cleared so that no residual silver halide remained. The minimum density in the clearest area was 0.6. This is too high for practical use.
  • a monobath composition for simultaneously developing and fixing an exposed photographic silver halide emulsion layer comprising an aqueous alkaline solution containing:
  • sufiicient thickening agent so that the viscosity of the monobath is from about 50 to about 20,000 centipoises at 24 C.
  • an amine compound which is either morpholine, a hydroxyalkyl amine containing a single hydroxyl group and wherein the hydroxyalkyl group has 1-5 carbon atoms, a sulfur dioxide addition product of morpholine or a sulfur dioxide addition product of said hydroxyalkyl amine.
  • R represents a hydroxyalkyl group having lcarbon atoms and R and R each represents a hydrogen atom or an alkyl hydrocarbon group having 1 to 3 carbon atoms.
  • said thickening agent is either a guar gum, carboxymethyl cellulose, hydroxyethyl cellulose, silica gel or starch.
  • a composition for processing an exposed photographic element comprising at least one silver halide emulsion layer and said element containing a photographic developing agent for reducing exposed silver halide to metallic silver, said composition comprising an aqueous alkaline solution containing (a) at least about 20 grams of a water-soluble thiosulfate per liter of solution,
  • sufiicient thickening agent so that the viscosity of the solution is from about 50 to about 20,000 centipoises at 24 C.
  • an amine compound which is either morpholine, a hydroxyalkyl amine containing a single hydroxyl group and wherein the hydroxyalkyl group has 1-5 carbon atoms, a sulfur dioxide addition product of morpholine or a sulfur dioxide addition product of said hydroxyalkyl amine.
  • a method of developing an exposed photographic silver halide emulsion layer using a monobath composition comprising a photographic silver halide developing agent for reducing exposed silver halide to metallic silver and sufficient water-soluble thiosulfate to fix substantially all unexposed silver halide, the improvement comprising adding to the monobath a small quantity of physical development nuclei; sufiicient thickening agent so that the viscosity of the monobath is from about 50 to about 20,000 centipoises at 24 C.; and an amine compound which is either morpholine, a hydroxyalkyl amine containing a single hydroxyl group and wherein the hydroxyalkyl group has -15 carbon atoms, a sulfur dioxide addition product of morpholine or a sulfur dioxide addition product of said hydroxyalkyl amine.
  • R represents a hydroxyalkyl group having 1-5 carbon atoms and R and R each represents a hydrogen atom or an alkyl hydrocarbon group having 1 to 3 carbon atoms.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
US590473A 1963-04-08 1966-10-31 Viscous silver halide photographid monobath solutions Expired - Lifetime US3392019A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
FR969478A FR1394373A (fr) 1963-04-08 1964-04-02 Nouveau bain de traitement photographique
BE646136A BE646136A (enrdf_load_stackoverflow) 1963-04-08 1964-04-03
DE19641447637 DE1447637A1 (de) 1963-04-08 1964-04-03 Photographischer Einbadentwickler zum gleichzeitigen Entwickeln und Fixieren von photographischen Silberhalogenidemulsionsschichten
GB14460/64A GB1066993A (en) 1963-04-08 1964-04-08 Photographic processing solutions
US590473A US3392019A (en) 1963-04-08 1966-10-31 Viscous silver halide photographid monobath solutions

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US27147863A 1963-04-08 1963-04-08
US590473A US3392019A (en) 1963-04-08 1966-10-31 Viscous silver halide photographid monobath solutions

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US3392019A true US3392019A (en) 1968-07-09

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BE (1) BE646136A (enrdf_load_stackoverflow)
DE (1) DE1447637A1 (enrdf_load_stackoverflow)
GB (1) GB1066993A (enrdf_load_stackoverflow)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3622332A (en) * 1968-04-19 1971-11-23 Itek Corp Photographic process with improved activator composition
US3765892A (en) * 1970-08-17 1973-10-16 Fuji Photo Film Co Ltd Viscous developer for silver halid diffusion transfer processes
US3767410A (en) * 1972-02-22 1973-10-23 Eastman Kodak Co Photographic hydrophilic colloids and method of coating
US3861919A (en) * 1970-03-30 1975-01-21 Itek Corp A photoconductor process using a copy medium sensitized with an amine
US4328304A (en) * 1978-09-22 1982-05-04 Fuji Photo Film Co., Ltd. Desensitizing solution for lithographic printing plate
US4351895A (en) * 1981-10-19 1982-09-28 American Hoechst Corporation Deletion fluid for positive printing plates
EP0619340A3 (en) * 1993-04-08 1995-07-05 Aqualon Co Thermally stable suspension of hydroxyethylcellulose in thiosulfate.

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE561545A (enrdf_load_stackoverflow) * 1956-10-29
US3120795A (en) * 1957-03-21 1964-02-11 Polaroid Corp Photographic products
CA682111A (en) * 1964-03-17 General Aniline And Film Corporation Combined developer and fixer bath
US3173789A (en) * 1962-01-29 1965-03-16 Eastman Kodak Co Method and composition for inhibiting silver sludge in thiosulfate monobaths
US3179517A (en) * 1959-08-24 1965-04-20 Eastman Kodak Co Web processing method and composition

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA682111A (en) * 1964-03-17 General Aniline And Film Corporation Combined developer and fixer bath
BE561545A (enrdf_load_stackoverflow) * 1956-10-29
US3120795A (en) * 1957-03-21 1964-02-11 Polaroid Corp Photographic products
US3179517A (en) * 1959-08-24 1965-04-20 Eastman Kodak Co Web processing method and composition
US3173789A (en) * 1962-01-29 1965-03-16 Eastman Kodak Co Method and composition for inhibiting silver sludge in thiosulfate monobaths

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3622332A (en) * 1968-04-19 1971-11-23 Itek Corp Photographic process with improved activator composition
US3861919A (en) * 1970-03-30 1975-01-21 Itek Corp A photoconductor process using a copy medium sensitized with an amine
US3765892A (en) * 1970-08-17 1973-10-16 Fuji Photo Film Co Ltd Viscous developer for silver halid diffusion transfer processes
US3767410A (en) * 1972-02-22 1973-10-23 Eastman Kodak Co Photographic hydrophilic colloids and method of coating
US4328304A (en) * 1978-09-22 1982-05-04 Fuji Photo Film Co., Ltd. Desensitizing solution for lithographic printing plate
US4351895A (en) * 1981-10-19 1982-09-28 American Hoechst Corporation Deletion fluid for positive printing plates
EP0619340A3 (en) * 1993-04-08 1995-07-05 Aqualon Co Thermally stable suspension of hydroxyethylcellulose in thiosulfate.

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BE646136A (enrdf_load_stackoverflow) 1964-07-31
DE1447637A1 (de) 1968-11-28
GB1066993A (en) 1967-04-26

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