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
  • G03C1/00—Photosensitive materials
  • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
  • G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
  • G03C1/08—Sensitivity-increasing substances
  • G03C1/10—Organic substances
  • G03C1/12—Methine and polymethine dyes
• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
  • G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
  • G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
  • G03C1/34—Fog-inhibitors; Stabilisers; Agents inhibiting latent image regression
  • G03C1/346—Organic derivatives of bivalent sulfur, selenium or tellurium
• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
  • G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
  • G03C2001/03564—Mixed grains or mixture of emulsions

Definitions

• the invention relates to a variable-grade black-and-white paper (BW paper) which contains at least two silver halide emulsions which are mixed prior to casting and which are sensitive to different spectral ranges, with a special stabilizer being added to at least one emulsion.
• BW paper black-and-white paper
• Gradation-variable light-sensitive silver halide materials contain emulsions that are light-sensitive for different spectral ranges. Depending on the composition of the copying light, a harder or softer gradation is achieved.
• the emulsions are usually mixed before pouring so that only one layer has to be poured. There is a danger that re-sensitization occurs, ie that the sensitizing dye is desorbed from the silver halide grains of an emulsion and adsorbed on grains of an unsensitized, blue-sensitive emulsion. This is undesirable, since a differentiated exposure by changing the Ko pierlichtes no longer leads to the desired result. Under unfavorable conditions, the process of sensitization is not limited to the casting solution, but can also occur on the finished material, for example under the influence of moisture, heat or both.
• the object of the invention was therefore to provide a gradation-variable SW paper in which these disadvantages do not occur.
• Suitable heterocyclic rings are 5- and 6-membered rings which contain one to three heteroatoms from the O, S, Se and N series and can be benzo- or naphtho-fused.
• Examples are oxazole, thiazole, selenazole, imidazole, tetrazole, triazoles, pyrimidine as well whose benzo and naphtho-fused derivatives by sulfo, carboxy, halogen, C1-C4-alkyl, aryl, especially phenyl, sulfophenyl, carboxyphenyl, C1-C4-alkylcarbonylamino, C1-C4-alkylaminosulfonyl or arylaminosulfonyl, especially phenylaminosulfonyl and chlorophenylaminosulfonyl can.
• R1 and R2 are the remaining members of a benzo or naphtho radical substituted by at least one solubilizing group, which may optionally contain further substituents.
• R1 and R2 are the remaining members of a benzo or naphtho radical substituted by one or two sulfo groups, which can be further substituted by C1-C4-alkyl or halogen.
• the sulfonic acid and mercapto groups can also be present in the form of their salts, in particular their alkali metal or ammonium salts. Suitable examples are:
• the emulsion with an absorption maximum between 480 and 580 nm is produced by conventional spectral sensitization with green-sensitive sensitizers.
• the emulsion with an absorption maximum below 480 nm is either an unsensitized silver halide emulsion, the intrinsic sensitivity of which is in the range given, absorptions below 360 nm are of no interest, since from here the absorption of the gelatin lies after shorter wavelengths, or an emulsion that contains a blue-sensitive sensitizer.
• the green and blue-sensitive partial emulsions can be mixed in a weight ratio of 1.5: 1 to 1:10, preferably 1: 1 to 1: 3, based on their silver content.
• the emulsions are preferably silver chloride bromide emulsions with 20 to 80 mol% chloride, 20 to 80 mol% bromide and 0 to 5 mol% iodide.
• the average grain size is in particular from 0.2 to 0.6 ⁇ m, the silver halide grains being cubic to octahedral.
• the average grain size can be between 0.2 to 0.6 ⁇ m, preferably 0.4 to 0.5 ⁇ m.
• the silver halide crystals can be doped with Rh3+, Ir4+, Cd2+, Zn2+, Pb2+.
• the emulsion can be desalted in the customary manner (dialysis, flocculation and redispersion, ultrafiltration).
• Chemical sensitization can take place through labile sulfur compounds (e.g. thiosulfate, diacetyl-thiourea), through gold-sulfur ripening or reduction ripening. Chemical sensitization can be carried out with the addition of Ir, Rh, Pb, Cd, Hg, Au.
• labile sulfur compounds e.g. thiosulfate, diacetyl-thiourea
• gold-sulfur ripening or reduction ripening e.g., gold-sulfur ripening or reduction ripening.
• Cyanine and merocyanine dyes as described in the monograph by F, M, Hamer, The Cyanine Dyes and Related Compounds, 1964, John Wiley & Sons, are suitable for producing the sensitivity in the range of 480-580.
• W2 C1-C4 alkyl, optionally substituted with hydroxy, carboxy or sulfo and Q are the ring members required to complete a rhodanine, thiohydantoin, thiooxazolidone or thiobarbituric acid ring.
• the second emulsion portion with a spectral sensitivity ⁇ 480 nm can also be used according to the invention without the addition of a spectral sensitizer, it is advantageous to increase this part of the emulsion in sensitivity at wavelengths ⁇ 480 nm by adding a suitable sensitizing dye.
• dyes of the following formulas are suitable for this purpose: wherein P the links required to supplement a benzo-fused heterocyclic five-membered ring R, T O, S, N-R7 R9, R10 CH3, CH3O, halogen and - if R or TO is - phenyl and Q, W1, W2, n, m have the meaning given above.
• the binder is an essential component of the at least one light-sensitive layer in addition to the silver halide.
• Gelatin is preferably used as the binder. However, this can be replaced in whole or in part by other synthetic, semi-synthetic or naturally occurring polymers.
• Synthetic gelatin substitutes are, for example, polyvinyl alcohol, poly-N-vinylpyrolidone, polyacrylamides, polyacrylic acid and their derivatives, in particular their copolymers.
• Naturally occurring gelatin substitutes are, for example, other proteins such as albumin or casein, cellulose, sugar, starch or alginates.
• Semi-synthetic gelatin substitutes are generally modified natural products.
• cellulose derivatives such as hydroxyalkyl cellulose, carboxymethyl cellulose and phthalyl cellulose and gelatin derivatives which have been obtained by reaction with alkylating or acylating agents or by grafting on polymerizable monomers.
• the binders should have a sufficient amount of functional groups, so that by reaction enough suitable layers can be produced with suitable hardening agents.
• functional groups are in particular amino groups, but also carboxyl groups, hydroxyl groups and active methylene groups.
• the gelatin which is preferably used can be obtained by acidic or alkaline digestion.
• the production of such gelatins is described, for example, in The Science and Technology of Gelatine, published by A.G. Ward and A. Courts, Academic Press 1977, page 295 ff.
• the gelatin used in each case should contain the lowest possible level of photographically active impurities (inert gelatin). High viscosity, low swelling gelatins are particularly advantageous.
• the silver halide present as a light-sensitive component in the photographic material can be predominantly compact crystals, which are e.g. are regular cubic or octahedral or can have transitional forms.
• platelet-shaped crystals may preferably also be present, the average ratio of diameter to thickness of which is preferably greater than 5: 1, the diameter of a grain being defined as the diameter of a circle with a circle content corresponding to the projected area of the grain.
• the silver halide grains can also have a multi-layered grain structure, in the simplest case with an inner and an outer grain area (core / shell), the halide composition and / or other modifications, such as doping of the individual grain areas, being different.
• the grain size distribution can be both homodisperse and heterodisperse. Homodisperse grain size distribution means that 95% of the grains do not deviate from the mean grain size by more than ⁇ 30%.
• the emulsions can also contain organic silver salts, for example silver benzotriazolate or silver behenate.
• Two or more kinds of silver halide emulsions, which are prepared separately, can be used as a mixture.
• the photographic emulsions can be prepared using various methods (e.g. P. Glafkides, Chimie et Physique Photographique, Paul Montel, Paris (1967), GF Duffin, Photographic Emulsion Chemistry, The Focal Press, London (1966), VL Zelikman et al, Making and Coating Photographic Emulsion, The Focal Press, London (1966) from soluble silver salts and soluble halides.
• various methods e.g. P. Glafkides, Chimie et Physique Photographique, Paul Montel, Paris (1967), GF Duffin, Photographic Emulsion Chemistry, The Focal Press, London (1966), VL Zelikman et al, Making and Coating Photographic Emulsion, The Focal Press, London (1966) from soluble silver salts and soluble halides.
• the silver halide is preferably precipitated in the presence of the binder, for example the gelatin, and can be carried out in the acidic, neutral or alkaline pH range, silver halide complexing agents preferably being additionally used.
• the latter include, for example, ammonia, thioether, imidazole, ammonium thiocyanate or excess halide.
• the water-soluble silver salts and the halides are optionally carried out in succession by the single-jet process or simultaneously by the double-jet process or by any combination of the two processes. Dosing with increasing inflow rates is preferred, the "critical" feed rate, at which no new germs are being produced, should not be exceeded.
• the pAg range can vary within wide limits during the precipitation, preferably the so-called pAg-controlled method is used, in which a certain pAg value is kept constant or a defined pAg profile is traversed during the precipitation.
• so-called inverse precipitation with an excess of silver ions is also possible.
• the silver halide crystals can also grow through physical ripening (Ostwald ripening), in the presence of excess halide and / or silver halide complexing agent.
• the growth of the emulsion grains can even take place predominantly by Ostwald ripening, preferably a fine-grained, so-called Lippmann emulsion, mixed with a less soluble emulsion and redissolved on the latter.
• the photographic emulsions can contain compounds for preventing the formation of fog or for stabilizing the photographic function during production, storage or photographic processing, in particular also in the layer which is sensitive in the range from 480 to 580 nm.
• Azaindenes are particularly suitable, preferably tetra- and penta-azaindenes, in particular those which are substituted by hydroxyl or amino groups. Such connections are for example from Birr, Z. Wiss. Phot. 47 (1952), pp. 2-58. Salts of metals such as mercury or cadmium, aromatic sulfonic or sulfinic acids such as benzenesulfinic acid, or nitrogen-containing heterocycles such as nitrobenzimidazole, nitroindazole, (subst.) Benzotriazoles or benzothiazolium salts can also be used as antifoggants.
• metals such as mercury or cadmium, aromatic sulfonic or sulfinic acids such as benzenesulfinic acid, or nitrogen-containing heterocycles such as nitrobenzimidazole, nitroindazole, (subst.) Benzotriazoles or benzothiazolium salts can also be used as
• Heterocycles containing mercapto groups for example mercaptobenzthiazoles, mercaptobenzimidazoles, mercaptotetrazoles, mercaptothiadiazoles, mercaptopyrimidines, are particularly suitable, these mercaptoazoles also being able to contain a water-solubilizing group, for example a carboxyl group or sulfo group.
• mercaptobenzthiazoles for example mercaptobenzthiazoles, mercaptobenzimidazoles, mercaptotetrazoles, mercaptothiadiazoles, mercaptopyrimidines
• these mercaptoazoles also being able to contain a water-solubilizing group, for example a carboxyl group or sulfo group.
• a water-solubilizing group for example a carboxyl group or sulfo group.
• the stabilizers can be added to the silver halide emulsions before, during or after their ripening.
• the compounds can also be added to other photographic layers which are assigned to a halogen silver layer.
• the photographic emulsion layers or other hydrophilic colloid layers of the light-sensitive material produced according to the invention can be surface-active Contain agents for various purposes, such as coating aids, to prevent electrical charging, to improve the sliding properties, to emulsify the dispersion, to prevent adhesion and to improve the photographic characteristics (e.g. acceleration of development, high contrast, sensitization, etc.).
• Chemical sensitization can take place through labile sulfur compounds (e.g. thiosulfate, diacetyl-thiourea), through gold-sulfur ripening or reduction ripening. Chemical sensitization can be carried out with the addition of Ir, Rh, Pb, Cd, Hg, Au, and addition of optical sensitizers or stabilizers is also possible.
• labile sulfur compounds e.g. thiosulfate, diacetyl-thiourea
• gold-sulfur ripening or reduction ripening e.g., gold-sulfur ripening or reduction ripening.
• Chemical sensitization can be carried out with the addition of Ir, Rh, Pb, Cd, Hg, Au, and addition of optical sensitizers or stabilizers is also possible.
• the photographic material may further contain UV light absorbing compounds, whites, spacers, formalin scavengers and others.
• Compounds that absorb UV light are intended on the one hand to protect the image dyes from fading by UV-rich daylight and, on the other hand, as filter dyes to absorb the UV light in daylight upon exposure and thus improve the color rendering of a film.
• Connections of different structures are usually used for the two tasks. Examples are aryl-substituted benzotriazole compounds (US Pat. No. 3,533,794), 4-thiazolidone compounds (US Pat. Nos. A3,314,794 and 3,352,681), benzophenone compounds (JP-A 2784/71), cinnamic acid ester compounds (US Pat. No. 3,705,805) and 3,707,375), butadiene compounds (US-A 4,045,229) or benzoxazole compounds (US-A 3,700,455).
• Ultraviolet absorbing couplers such as ⁇ -naphthol type cyan couplers
• ultraviolet absorbing polymers can also be used. These ultraviolet absorbents can be fixed in a special layer by pickling.
• Suitable white toners are e.g. in Research Disclosure December 1978, page 22 ff, Unit 17 643, Chapter V.
• the average particle diameter of the spacers is in particular in the range from 0.2 to 10 ⁇ m.
• the spacers are water-insoluble and can be alkali-insoluble or alkali-soluble, the alkali-soluble ones generally being removed from the photographic material in the alkaline development bath.
• suitable polymers are polymethyl methacrylate, copolymers of acrylic acid and methyl methacrylate and hydroxypropyl methyl cellulose hexahydrophthalate.
• binders of the material according to the invention are hardened with suitable hardeners, for example hardeners of the epoxy type, the ethyleneimine type, the acryloyl type or the vinylsulfone type. Diazine, triazine or 1,2-dihydroquinoline series hardeners are also suitable.
• the binders of the material according to the invention are preferably hardened with instant hardeners.
• Immediate hardeners are understood to mean compounds which crosslink suitable binders in such a way that the hardening is completed to such an extent immediately after casting, at the latest after 24 hours, preferably at the latest after 8 hours, that no further change in the sensitometry caused by the crosslinking reaction and the swelling of the layer structure occurs .
• Swelling is understood to mean the difference between the wet film thickness and the dry film thickness during the aqueous processing of the film (Photogr. Sci. Eng. 8 (1964), 275; Photogr. Sci. Eng. (1972), 449).
• hardening agents that react very quickly with gelatin are e.g. to carbamoylpyridinium salts, which are able to react with free carboxyl groups of the gelatin, so that the latter react with free amino groups of the gelatin to form peptide bonds and crosslink the gelatin.
• Suitable examples of instant hardeners are, for example, compounds of the general formulas wherein R1 denotes alkyl, aryl or aralkyl, R2 has the same meaning as R1 or means alkylene, arylene, aralkylene or alkaralkylene, the second bond having a group of the formula is linked, or R1 and R2 together represent the atoms required to complete an optionally substituted heterocyclic ring, for example a piperidine, piperazine or morpholine ring, which ring can be substituted, for example, by C1-C3alkyl or halogen, R3 for hydrogen, alkyl, aryl, alkoxy, -NR4-COR5, - (CH2) m -NR8R9, - (CH2) n -CONR13R14 or or a bridge link or a direct bond to a polymer chain, wherein R4, R6, R7, R9, R14, R15, R17, R18, and R19 are hydrogen
• the materials according to the invention are processed in the usual manner according to the processes recommended for this.
• Grain diameter 0.42 microns is desalted in a known manner and matured after the addition of 20 microns thiosulfate / mole AgNo3 under sensitometric control to an optimal sensitivity-fog ratio.
• the emulsion contains 100 g of AgNO3 in 1 kg of emulsion.
• Green-sensitized partial emulsion 300 g of the emulsion are optically sensitized for the green spectral range by adding 37 mg of the sensitizer SE 18 and stabilized by adding 30 mg of 5-hydroxy-7-methyl-1,3,8-triazaindolizine per kg of emulsion.
• Unsensitized partial emulsion 700 g of the emulsion are stabilized by adding 30 mg of 5-hydroxy-7-methyl-1,3,8-triazaindolizine.
• the partial emulsions are mixed; a part is cast on an opaque support with the addition of a gelatin hardening agent (experiment 1A). Another part of the mixture is kept at 40 ° C. for 4 hours and then poured with the addition of a gelatin hardening agent (experiment 1B).
• Emulsion preparation and sensitization for the spectral range from 480 to 580 nm is carried out according to Example 1.
• Unsensitized partial emulsion This part of the emulsion is stabilized as in Example 1 with 30 mg 5-hydroxy-7-methyl-1,3,8-triazaindolizine and additionally with 200 mg Stabilizer III per kg emulsion.
• the partial emulsions are mixed and poured according to Example 1 (tests 2A and 2B).
• Emulsion preparation and sensitization for the spectral range from 480 to 580 nm correspond to Example 1, but 250 g of an emulsion of 60 mol% AgCl, 39.5 mol% AgBr and 0.5 mol% AgI are used.
• Blue-sensitized partial emulsion 250 mg of the unsensitized emulsion are mixed with 20 mg of sensitizer BS6 and 30 mg of 5-hydroxy-7-methyl-1,3,8-triazaindolizine.
• Unsensitized partial emulsion 500 g of the unsensitized emulsion are mixed with 30 mg of 5-hydroxy-7-methyl-1,3,8-triazaindolizine and 160 mg of stabilizer I.
• a sample of the material is exposed behind a yellow filter and a step part.
• a second sample is exposed behind a purple filter and a step part.
• the developer is then developed with a developer customary for SW paper (e.g. Agfa 100) and the density of the steps is measured.
• Log ER is determined from the density curve in accordance with ANSI standard PH 2.2-1966 (Table 1).
• a part of the material (1A, 2A, 3A) is subjected to an artificial aging by storage for 2 days in a warm, humid atmosphere at 45 ° C. and 65% rel. Moisture (1C, 2C, 3C).
• Example 3 Yellow filter: 1A 1.20 2A 1.25 3A 1.38 1B 0.95 2 B 1.20 3B 1.35 Purple filter: 1A 0.60 2A 0.58 3A 0.56 1B 0.75 2 B 0.62 3B 0.60 he lied example 1
• Example 3 Yellow filter: 1A 1.20 2A 1.25 3A 1.38 1C 1.05 2C 1.20 3C 1.34 Purple filter: 1A 0.60 2A 0.58 3A 0.56 1C 0.70 2C 0.61 3C 0.59
• the examples according to the invention each show the slightest changes.
• Example 2 Analogously to Example 1, the following emulsions of the specified composition and grain size are prepared and chemically ripened. Each emulsion is divided into 2 equal parts, of which the first partial emulsion is sensitized with the spectral sensitizer in the range between 480 and 580 nm and the second partial emulsion is mixed with the stabilizer according to the invention. Then the two partial emulsions are mixed and cast as usual on PR paper base with an application of 1.4 g of silver per m2. These samples according to the invention are designated A.
• Samples B differ from A in that the stabilizer in the second partial emulsion is omitted.
• Samples C contain the spectral sensitizer evenly distributed on all emulsion crystals in the same concentration per m2 as in samples A and B.
• the samples are then subjected to sensitometric exposure behind a yellow and a purple filter with the spectral characteristics "Gb" and "Pp" shown in FIG. 1. It is then developed in Agfa-Neutol paper developer and log ER determined.
• a silver chloride emulsion with 70 mol% chloride and 30 mol% bromide and an average grain size of 0.3 ⁇ is produced and chemically ripened as described in Example 1.
• the emulsion is then divided into two equal parts as described in Example 4.
• the first partial emulsion is sensitized with 75 ⁇ mol per mole Ag of the sensitizer dye SE 6.
• the second partial emulsion is sensitized with a blue sensitizer BS as indicated in Table 6 and stabilized with 240 mg of stabilizer III.
• the part emulsions After the part emulsions have been mixed, they are poured onto PE paper substrates. As in Example 4, the layers are subjected to sensitometric exposure behind a yellow and purple filter.
• the blue sensitivity (column 5) can be increased considerably by adding the blue sensitizers without losing the gamma differentiation according to the invention.

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• Chemical & Material Sciences (AREA)
• Physics & Mathematics (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• General Physics & Mathematics (AREA)
• Spectroscopy & Molecular Physics (AREA)
• Crystallography & Structural Chemistry (AREA)
• Silver Salt Photography Or Processing Solution Therefor (AREA)
• Paper (AREA)
• Plural Heterocyclic Compounds (AREA)
• Ink Jet Recording Methods And Recording Media Thereof (AREA)

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• 1987
  • 1987-11-24 DE DE19873739766 patent/DE3739766A1/de not_active Withdrawn
• 1988
  • 1988-11-10 US US07/269,993 patent/US5006455A/en not_active Expired - Fee Related
  • 1988-11-17 EP EP88119074A patent/EP0317886B1/fr not_active Expired - Lifetime
  • 1988-11-17 ES ES88119074T patent/ES2050139T3/es not_active Expired - Lifetime
  • 1988-11-17 DE DE88119074T patent/DE3888461D1/de not_active Expired - Fee Related
  • 1988-11-17 JP JP63289025A patent/JP2622407B2/ja not_active Expired - Fee Related

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