US3765889A - Silver transfer diffusion process - Google Patents

Silver transfer diffusion process Download PDF

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US3765889A
US3765889A US00130383A US3765889DA US3765889A US 3765889 A US3765889 A US 3765889A US 00130383 A US00130383 A US 00130383A US 3765889D A US3765889D A US 3765889DA US 3765889 A US3765889 A US 3765889A
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silver halide
silver
stratum
film unit
mercapto
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R Young
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Polaroid Corp
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Polaroid Corp
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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
    • G03C8/00—Diffusion transfer processes or agents therefor; Photosensitive materials for such processes
    • G03C8/02—Photosensitive materials characterised by the image-forming section
    • G03C8/04—Photosensitive materials characterised by the image-forming section the substances transferred by diffusion consisting of inorganic or organo-metallic compounds derived from photosensitive noble metals
    • G03C8/06—Silver salt diffusion transfer

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  • This invention relates, in general, to diffusion transfer photography and, more particularly, to silver diffusion transfer processes.
  • a primary object of this invention is to provide diffusion transfer processes employing regenerated cellulose silver-receptive strata wherein the silver transfer image exhibits improved highlights.
  • a further object of this invention is to provide silver diffusion transfer processes, and products useful in performing such processes, wherein the photosensitive silver halide emulsion contains silver halide grains of specified character whereby improved silver transfer images may be obtained.
  • the invention accordingly comprises the process involving the several steps and the relation and order of one or more of such steps with respect to each of the others, and the products possessing the features, properties and the relation of elements which are exemplified in the following detailed disclosure, and the scope of the application of which will be indicated in the claims.
  • FIG. 1 reproduces a graph of the grain size distribution of a silver halide emulsion found to be useful in accordance with this invention and compared with a control silver halide emulsion;
  • FIG. 2 reproduces graphs of the grain size distribution, area and volume of a silver halide emulsion found useful in accordance with this invention.
  • FIG. 3 reproduces graphs of the type shown in FIG. 2 and plotted with respect to a control silver halide emulsion.
  • a photoexposed silver halide material and a silver precipitating material are subjected to an aqueous alkaline solution comprising at least a silver halide developing agent and a silver halide solvent.
  • the developing agent reduces exposed silver halide to silver and the solvent reacts with unreduced silver halide to form a complex silver salt that migrates to the silver precipitating material where it is precipitated or reduced to form a visible silver image.
  • said copending Land application discloses diffusion transfer processes employing imagereceiving elements prepared by incorporating a silver precipitating agent in an alkali-impermeable polymer or polymeric material to provide a dispersion wherein said silver precipitating agent constitutes the inner phase of said dispersion.
  • the resulting dispersion is then coated as a layer on a support and subjected to appropriate hydrolysis treatment to convert at least a depthwise portion of said alkali-impermeable polymer to an alkali-permeable polymer.
  • the hydrolyzed polymer in which the silver transfer image is formed is water-insoluble, as in the case of regenerated cellulose obtained by hydrolysis of cellulose diacetate, the resulting transfer image may be subjected to washing without danger of physical damage, the washed print exhibiting high gloss and exceptional stability characteristics.
  • This invention is concerned with improvements in diffusion transfer processes employing image-receiving elements of the type described in said Land application, and to improve the photographic and optical properties of the silver transfer image formed in said image-receiving element.
  • silver transfer images formed in regenerated cellulose exhibit advantageous handling and stability characteristics. Particularly good image stability properties are obtained when the process is performed using a hydroxylamine silver halide developing agent and an organic silver halide solvent, the resulting silver transfer images exhibiting exceptional stability without requiring washing or print coating. It has been found, however, that longer imbibition times may be necessary to reach a desired maximum density, e.g., a density of about 1.4 to 1.6, than is the case with prior silver transfer processes employing benzenoid silver halide developing agents and inorganic silver halide solvents.
  • a desired maximum density e.g., a density of about 1.4 to 1.6
  • the silver halide solvent may dissolve and transfer silver halide grains that would have been developed with a shorter induction period developing agent, thereby increasing highlight density. It has now been found that undesired minimum density may be avoided by employing a silver halide emulsion having particular silver halide grain characteristics as hereinafter set forth in detail.
  • Hydroxylamine silver halide developing agents have been found to be particularly useful in forming silver transfer images which require little or no after treatment, especially when used in combination with regenerated cellulose silver receptive strata.
  • Particularly useful hydroxylamine silver halide developing agents are the N-alkyl and N-alkoxyalkyl substituted hydroxylamines. A large number of such hydroxylamines are described in U. S. Pat. Nos. 2,857,274, 2,857,275 2,857,276, 3,287,124, 3,287,125 and 3,293,034.
  • Particularly effective and preferred hydroxylamine silver halide developing agents may be described by the formula wherein R is alkyl, alkoxyalkyl or alkoxyalkoxyalkyl, and R is hydrogen, alkyl, alkoxyalkyl, alkoxyalkoxyalkyl or alkenyl.
  • the alkyl, alkoxy and alkenyl. radicals preferably contain from one to three carbons.
  • Particularly useful hydroxylamine silver halide developing agents include N,N-diethyl-hydroxylamine, N,N-bismethoxyethyl-hydroxylamine and N,N-bis-ethoxyethylhydroxylamine.
  • the silver halide solvent may be an alkali metal thiosulfate, e.g., sodium or potassium thiosulfate, and preferably is a cyclic imide of the type discussed in detail in the aforementioned U.S. Pat. Nos. 3,857,274, 2,857,275 and 3,857,276, e.g., uracil, urazole, 5- methyl-uracil, etc.
  • the processing composition includes an alkali, preferably an alkali metal hydroxide such as sodium or potassium hydroxide. If the processing composition is applied by being distributed as a thin layer between the superposed photosensitive ad image-receiving elements, and particularly if so distributed as said elements, are brought into superposed relationship, the processing composition preferably includes a polymeric film-forming, thickening or viscosity-providing agent. I-Iydroxyethyl cellulose and sodium carboxymethyl cellulose are particularly useful for this purpose, and are included in the processing composition in concentrations effective to provide the appropriate viscosity in accordance with principles well-known in diffusion transfer photography.
  • an alkali preferably an alkali metal hydroxide such as sodium or potassium hydroxide.
  • the processing composition may also include other additives, as is conventional in silver transfer processes, such as anitfoggants, toning agents, stabilizing agents, etc.
  • additives such as anitfoggants, toning agents, stabilizing agents, etc.
  • an oxyethylamino compound such as triethanolamine, to increase the processing composition shelf life as disclosed and claimed in the copending application of Sidney Kasman, Ser. No. 725,145 filed Apr. 29, 1968 (now U. S. Pat. No. 3,619,185 issued Nov. 9, 1971).
  • the unhydrolyzed portion of the cellulose ester layer containing a silver precipitating agent and/or an underlying unhydrolyzed cellulose ester, e.g., cellulose diacetate contain one or more mercapto compounds adapted to improve the tone, stability, or other photographic property of the silver transfer image; such mercapto compounds are made available during imbibition by diffusion from their initial location.
  • Image-receiving elements of this type are disclosed and claimed in the copending application of Richard W. Young, Ser. No. 717,683 filed Apr. 1, 1968 (now U. S. Pat. No. 3,607,269 issued Sept. 21, 1971).
  • suitable silver precipitating agents include heavy metals such as iron, lead, zinc, nickel, cadmium, tin, chromium, copper, cobalt, particularly noble metals such as gold, silver, platinum and palladium.
  • Other useful silver precipitating agents include sulfides and selenides of heavy metals, particularly: sulfides of mercury, copper, aluminum, zinc, cadmium, cobalt, nickel, silver, lead, antimony, bismuth, cerium and magnesium; and selenides of lead, zinc, antimony and nickel.
  • the function of such materials as silver precipitating agents in a silver transfer process is described, for example, in U.S. Pat. No. 2,774,667, issued on Dec. 18, 1956 in the names of Edwin H. Land et al.
  • the silver halide emulsions found to give improved minimum density silver transfer images in accordance with this invention comprise silver bromide, silver iodobromide or other mixed halide emulsions wherein the silver halide is substantially completely in the form of silver halide grains having a diameter of at least 0.5 micron, i.e., at least and preferably at least 99%, of the silver halide grains have a diameter of at least 0.5 micron.
  • Grain size distribution curves or grain size-frequency distribution curves as they are sometimes called, are frequently used to describe and define silver halide emulsions.
  • Mees and James The Theory of the Photographic Process, 3rd Edition, The Macmillan Company, New York, N.Y. 1966, pages 36-44, set forth a description of techniques of measuring the size of silver halide grains and of determining the frequency of grains of given sizes in a particular silver halide emulsion.
  • Electron microscope size-frequency analysis of silver halide emulsions gives very high accuracy measurements, particularly of grains below the resolution of light microscopy but is a relatively slow procedure.
  • Emulsion B the silver halide emulsion having the grain size distribution depicted in curve B and wherein substantially all of the silver is present of the form of grains having a diameter of approximately 0.5 micron and larger.
  • Emulsion B the silver halide emulsion
  • FIGS. 2 and 3 depict grain size distribution curves N of data obtained by electron microscopy for different samples of the above Emulsions A and B, respectively, as well as area curves NA and volume curves NV for the same emulsions.
  • the horizontal axis for each of the curves in FIGS. 2 and 3 represents relative log diameter of the silver halide grains, while the vertical axis represents the number of grains normalized, with the dotted curves representing cumulative percentile; the 0.5 micron point as marked on the horizontal axes and the 50th percentile point is marked on the vertical axes.
  • the NA curves depict how much of the total area covered is represented by grains of a given size, while the NV curves depict how much of the total silver present is represented by grains of a given size.
  • the cumulative percentile values for N, Na And NV for representative grain diameters of Emulsions A and B found in the electron microscopy analysis were:
  • Emulsion B is substantially completely in the form of grains having a diameter of more than 0.5 micron.
  • Emulsion A and Emulsion B are gelatino silver iodobromide emulsions containing 6 mole percent iodide, with a gelatin to silver ratio of 2.5.
  • the emulsions were coated at levels of approximately 100 mg. of silver per square foot.
  • Emulsion B defined above was coated on a support to provide a silver coverage of approximately 99 mg.
  • the resulting photosensitive element was photoexposed and then diffusion transfer processed by distributing a layer 0.0028 inch thick of a processing composition between said photoexposed silver halide emulsion and a regenerated cellulose imagereceiving element.
  • the processing composition comprised:
  • Potassium hydroxide (aqueous solution 45% KOH) 323 cc. Titanium dioxide 3 g. l-lydroxyethyl cellulose 79 g. Zinc oxide 9.75 g. N,N-bis-methoxyethylhydroxylamine g. Triethanolamine solution (4.5 parts triethanolamine to 6.2 parts water) 17.14 g. Tetrahydropyrimidine thione 0.4 g. 2,4-dimercaptopyrimidine 0.35 g. Uracil g. Water 1193 cc.
  • the image-receiving element was prepared by coating baryta paper with a 0.25 mil layer of cellulose diacetate (2.4 DS) containing mg. per square foot of 1,6-bis- (5-mercapto-1,3 ,4-thiadizaolyl-2-thio)-hexane followed by a 0.2 mil layer of cellulose diacetate (2.4 DS) containing colloidal nickel sulfide as silver precipitating agent and 50 mg. per square foot of 1,6-bis-(5- mercapto-1,3 ,4-thiadiazolyl-2-thio-hexane, after which the outer cellulose acetate layer was hydrolyzed to regenerated cellulose to a depth of approximately 0.075 mil. After a 30 second inbibition, the image-receiving element was separated and contained a high quality silver transfer image with a maximum density of 1.48 and a minimum density of 0.04, with a Diffusion Transfer Equivalent Exposure Index of 3400.
  • EXAMPLE 2 The process set forth in Example 1 was repeated, replacing the tetrahydropyrimidine thione with 0.15g'. per liter of imidazolidine-Z-thione. The resulting silver transfer image exhibited comparable minimum and maximum densities, a more neutral tone and higher contrast compared with the silver transfer image obtained in Example 1.
  • EXAMPLE 3 For comparison purposes, a photosensitive element having silver halide Emulsion A coated at .approximately 100 mg. per square foot was processed in the same manner as described in Example 1. The resulting silver transfer image also had a minimum density of 0.04 but the maximum density had dropped to 1.22 and the Diffusion Transfer Equivalent Exposure Index was 2900. By increasing the nickel sulfide concentration in the image-receiving layer three-fold, the maximum density of the silver transfer image was increased to the level obtained in Example 1 but the minimum density almost doubled to 0.07. This comparison illustrates the reduction in minimum density obtained without loss of maximum density by use of a silver halide emulsion having the silver halide substantially completely in the form of grains having a diameter of at least 0.5 micron.
  • transparent supports may be employed in lieu of paper supports where it is desired to have transparencies which may be viewed by transmitted light or by projection. It is also within the scope of this invention to use a translucent support, e.g., a cellulose acetate support which has been ocated with a translucent layer of titanium dioxide. Use of a translucent support permits the transfer image to be viewed by reflected or transmitted light.
  • a thin strip coat e.g., of dimethyl hydantoin formaldehyde or gum arabic
  • the strip coat may also serve as a carrier for a reagent, e.g., a toning agent; in that event, a portion of such reagent may also diffuse inwardly into the hydrolyzed layer.
  • the photographic processing solution is effective to extract alkali-soluble reagents from the unhydrolyzed polymer and diffuse them into the hydrolyzed stratum during photographic processing. It is also possible to effect a redistribution of such alkali-soluble reagents from the unhydrolyzed to the hydrolyzed stratum prior to photographic processing by briefly contacting the image-receiving element with a solution such as aqueous methanol, with or without an alkali also being present.
  • Mercapto-thiadiazoles e.g., Z-acetamido-S-mercapto-l ,3,4-thiadiazole and 1,6-bis-(-mercapto-1,3 ,4- thiadiazolyl-Z-thio )-hexane, give unexpectedly superior results in increasing the stability of silver transfer images to attack, and especially to attack by sulfur.
  • the pre-imbibition hydrolysis is of only a portion of the image-receiving layer
  • the silver precipitating nuclei are present in both the hydrolyzed and unhydrolyzed portions of this layer.
  • Examination of photomicrographs of cross-sections of such partially hydrolyzed cellulose acetate receiving layers has shown that the transfer image silver is deposited only in the pre-imbibition hydrolyzed portion, even though a substantial portion of the originally unhydrolyzed cellulose acetate may be hydrolyzed by a secondary hydrolysis during imbibition and silver precipitating nuclei thus made available deeper in the imagereceiving element.
  • the cellulose acetate has been hydrolyzed to a depth of about 0.00002 to 0.00015 inches, the total thickness of the hydrolyzed and unhydrolyzed portions being about 0.00010 to 0.00050 inches, these thicknesses being measured after hydrolysis (and prior to diffusion transfer processing) since some shrinking of the original coated thickness will occur as a result of the hydrolysis and subsequent heat drying.
  • the hydrolyzed portion is about 0.00004 to 0.00010 inches and the total thickness of the hydrolyzed and unhydrolyzed portions is about 0.00015 to 0.00030 inches.
  • the total thickness prior to hydrolysis may be about 0.00015 to 0.00060 inches, and preferably about 0.00020 to 0.00030 inches.
  • silver precipitants are present in very low quantities, e.g., about 1 to 25 X moles per square foot. The lowest possible levels are usually used, as higher concentrations may cause excessive silver deposition or undesirable background density in the highlight areas. Mixtures of silver precipitants may be used.
  • the image-receiving layer thus may be described as substantially colorless and substantially transparent insofar as the presence of the nuclei is concerned.
  • the hydrolyzed polymer exhibits an adhesive tendency towards the solidified layer of processing fluid, e.g., as may occur where the surface of the image-receiving element is converted to cellulose and the processing fluid contains a film-forming polymer such as sodium carboxymethyl cellulose or hydrolyzed surface with a suitable stripping layer to facilitate separation of the image-receiving element from the layer of processing fluid.
  • a film-forming polymer such as sodium carboxymethyl cellulose or hydrolyzed surface with a suitable stripping layer to facilitate separation of the image-receiving element from the layer of processing fluid.
  • Materials suitable for providing a stripping layer are well known in the art, and are exemplified by materials such as cellulose acetate hydrogen phthalate as well as others mentioned above. it will be appreciated, however, that in some instances it may be desirable to have the solidified layer of processing fluid preferentially adhere to the surface of such an image-receiving layer, in which event such a stripping layer should be omitted.
  • Additive color images may be formed by forming the silver transfer image in accordance with this invention, said image being in registered relationship with an additive color screen.
  • the additive color screen is preferably positioned between a transparent support and said silver-receptive stratum, exposure of the silver halide emulsion being effected through said screen.
  • the silver halide emulsion may be coated over the image-receptive stratum, the silver halide emulsion being removable after processing, as by provision of a suitable stripping layer or by employment of a silver halide emulsion which may be readily washed off after processing, e.g., a silver halide emulsion wherein the binder is cellulose acetate hydrogen phthalate.
  • a pigmented layer e.g., titanium dioxide in gelatin or a suitable plastic, may be positioned between the silver halide emulsion and the silver-receptive stratum coated on a transparent base, and the silver transfer image viewed through the transparent base against the pigmented layer, the pigmented layer masking out the image in the developed silver halide emulsion layer.
  • the method of forming asilver transfer image comprising exosing a photosensitive silver halide emulsion, developing said exposed silver halide emulsion with an aqueous alkaline processing solution including a hydroxylamine silver halide developing agent and a silver halide solvent, forming an imagewise distribution of a diffusible silver complex as a function of said development, transferring at least a portion of said imagewise distribution of diffusible silver complex to a superposed silver receptive stratum of regenerated cellulose containing a silver precipitating agent to form said silver transfer image, the silver halide of said silver halide emulsion being substantially completely in the form of grains having a diameter of at least 0.5 micron.
  • said silver halide developing agent is an N,N-bis-alkoxyalkylhydroxylamine wherein each of said alkoxy and alkyl radicals contain from one to three carbons.
  • said silver halide developing agent is an N,N-dialky1 substituted hydroxylamine and said silver halide solvent is a cyclic imide.
  • said silver precipitating agent is a colloidal metal sulfide.
  • a diffusion transfer film unit comprising a photosensitive silver halide emulsion in which the silver halide is substantially completely in the form of grains having a diameter greater than 0.5 microns, an image receiving layer comprising a stratum of regenerated cellulose containing a silver precipitating agent, and a processing composition comprising an aqueous alkaline solution, said film unit including a hydroxylamine silver halide developing agent and a silver halide solvent, said photosensitive silver halide emulsion and said image receiving layer being carried by a single support or being carried by separate superposable supports.
  • a film unit as defined in claim 13 wherein said silver halide developing agent is an N,N-bis-alkoxyalkylhydroxylamine wherein each of the alkoxy and alkyl radicals contains from one to three carbon atoms.
  • a film unit as defined in claim 20 wherein said mercapto substituted compound is a mercaptothiadiazole.
  • a diffusion transfer film unit comprising a first support carrying a photosensitive silver halide emulsion wherein less than 1% of the silver halide grains have a diameter less than 0.5 microns, a second support carrying an image receiving layer comprising a stratum of regenerated cellulose containing silver precipitating agent contiguous with a stratum of alkali hydrolysable cellulose ester, and a rupturable container releasably holding a processing composition comprising an aqueous alkaline solution, an N,N-dialkyl substituted hydroxylamine silver halide developing agent and an organic silver halide solvent, said rupturable container being so positioned as to discharge its contents for distribution between said silver halide emulsion and said image-receiving layer.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Photosensitive Polymer And Photoresist Processing (AREA)
US00130383A 1971-04-01 1971-04-01 Silver transfer diffusion process Expired - Lifetime US3765889A (en)

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US (1) US3765889A (fr)
JP (1) JPS5529417B1 (fr)
AU (1) AU451556B2 (fr)
BE (1) BE781475A (fr)
CA (1) CA979264A (fr)
DE (1) DE2215788C2 (fr)
FR (1) FR2132095B1 (fr)
GB (1) GB1381548A (fr)
IT (1) IT952356B (fr)
NL (1) NL171632C (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3864131A (en) * 1972-12-25 1975-02-04 Fuji Photo Film Co Ltd Developer for silver salt diffusion transfer photography
US4298677A (en) * 1979-06-07 1981-11-03 Fuji Photo Film Co., Ltd. Diffusion transfer photographic process
US4659646A (en) * 1984-06-18 1987-04-21 Fuji Photo Film Co., Ltd. Silver salt diffusion transfer photographic material
US5308738A (en) * 1991-06-20 1994-05-03 Agfa-Gevaert, N.V. Silver salt diffusing transfer material with light insensitive silver salt layer

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4278756A (en) * 1979-07-06 1981-07-14 Drexler Technology Corporation Reflective data storage medium made by silver diffusion transfer
EP0557616A1 (fr) * 1992-02-07 1993-09-01 Agfa-Gevaert N.V. Un matériau à halogénure d'argent utilisable dans un procédé de diffusion-transfert du sel d'argent

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2662822A (en) * 1949-04-21 1953-12-15 Polaroid Corp Photographic transfer processes and compositions for the practice of said processes
US3031304A (en) * 1958-08-20 1962-04-24 Albert J Oliver Fine grain nuclear emulsion
US3501305A (en) * 1966-03-11 1970-03-17 Eastman Kodak Co Monodispersed photographic reversal emulsions
US3687677A (en) * 1966-05-31 1972-08-29 Eastman Kodak Co Photosensitive elements having high surface concentration of silver halide and stabilized against contamination fog

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3293034A (en) * 1963-06-26 1966-12-20 Polaroid Corp Alkoxy hydroxylamines as photographic developers
GB1082012A (en) * 1964-05-23 1967-09-06 Kodak Ltd Sensitive photographic materials and emulsions therefor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2662822A (en) * 1949-04-21 1953-12-15 Polaroid Corp Photographic transfer processes and compositions for the practice of said processes
US3031304A (en) * 1958-08-20 1962-04-24 Albert J Oliver Fine grain nuclear emulsion
US3501305A (en) * 1966-03-11 1970-03-17 Eastman Kodak Co Monodispersed photographic reversal emulsions
US3687677A (en) * 1966-05-31 1972-08-29 Eastman Kodak Co Photosensitive elements having high surface concentration of silver halide and stabilized against contamination fog

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Photographic Science and Engineering, Vol. 5, No. 6, November December 1961, pp. 332 336 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3864131A (en) * 1972-12-25 1975-02-04 Fuji Photo Film Co Ltd Developer for silver salt diffusion transfer photography
US4298677A (en) * 1979-06-07 1981-11-03 Fuji Photo Film Co., Ltd. Diffusion transfer photographic process
US4659646A (en) * 1984-06-18 1987-04-21 Fuji Photo Film Co., Ltd. Silver salt diffusion transfer photographic material
US4677052A (en) * 1984-06-18 1987-06-30 Fuji Photo Film Co., Ltd. Silver salt diffusion transfer photographic material comprising fine and coarse grain silver halide
US5308738A (en) * 1991-06-20 1994-05-03 Agfa-Gevaert, N.V. Silver salt diffusing transfer material with light insensitive silver salt layer

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DE2215788C2 (de) 1982-12-09
CA979264A (en) 1975-12-09
DE2215788A1 (de) 1972-10-12
NL171632C (nl) 1983-04-18
IT952356B (it) 1973-07-20
BE781475A (fr) 1972-10-02
FR2132095B1 (fr) 1977-04-01
GB1381548A (en) 1975-01-22
NL7204161A (fr) 1972-10-03
AU451556B2 (en) 1974-07-15
NL171632B (nl) 1982-11-16
AU3940472A (en) 1973-08-30
JPS5529417B1 (fr) 1980-08-04
FR2132095A1 (fr) 1972-11-17

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