EP0651284A1 - Fällung von Silberhalogenidkristallen, die lodid enthalten - Google Patents
Fällung von Silberhalogenidkristallen, die lodid enthalten Download PDFInfo
- Publication number
- EP0651284A1 EP0651284A1 EP93203040A EP93203040A EP0651284A1 EP 0651284 A1 EP0651284 A1 EP 0651284A1 EP 93203040 A EP93203040 A EP 93203040A EP 93203040 A EP93203040 A EP 93203040A EP 0651284 A1 EP0651284 A1 EP 0651284A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- iodide
- silver
- group
- crystals
- emulsion
- 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- Withdrawn
Links
- -1 silver halide Chemical class 0.000 title claims abstract description 107
- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 66
- 239000004332 silver Substances 0.000 title claims abstract description 66
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000001556 precipitation Methods 0.000 title description 46
- 239000000839 emulsion Substances 0.000 claims abstract description 104
- 239000000243 solution Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 46
- 238000012545 processing Methods 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910001507 metal halide Inorganic materials 0.000 claims abstract description 6
- 150000005309 metal halides Chemical class 0.000 claims abstract description 6
- 125000005647 linker group Chemical group 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 150000004820 halides Chemical class 0.000 claims description 15
- JDNTWHVOXJZDSN-UHFFFAOYSA-N iodoacetic acid Chemical group OC(=O)CI JDNTWHVOXJZDSN-UHFFFAOYSA-N 0.000 claims description 10
- 239000004848 polyfunctional curative Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 125000004429 atom Chemical group 0.000 claims description 4
- QZRGKCOWNLSUDK-UHFFFAOYSA-N Iodochlorine Chemical compound ICl QZRGKCOWNLSUDK-UHFFFAOYSA-N 0.000 claims description 3
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims description 3
- 238000011069 regeneration method Methods 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 125000002252 acyl group Chemical group 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 claims description 2
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 2
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 2
- 125000005842 heteroatom Chemical group 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 125000005702 oxyalkylene group Chemical group 0.000 claims description 2
- 125000005740 oxycarbonyl group Chemical group [*:1]OC([*:2])=O 0.000 claims description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 41
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 40
- 239000000975 dye Substances 0.000 description 30
- 239000010410 layer Substances 0.000 description 28
- 150000001875 compounds Chemical class 0.000 description 27
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 25
- 206010070834 Sensitisation Diseases 0.000 description 20
- 230000008313 sensitization Effects 0.000 description 20
- 108010010803 Gelatin Proteins 0.000 description 19
- 239000003795 chemical substances by application Substances 0.000 description 19
- 239000008273 gelatin Substances 0.000 description 19
- 229920000159 gelatin Polymers 0.000 description 19
- 235000019322 gelatine Nutrition 0.000 description 19
- 235000011852 gelatine desserts Nutrition 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 17
- 230000035945 sensitivity Effects 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 230000003595 spectral effect Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 239000011258 core-shell material Substances 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 239000000084 colloidal system Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 230000001681 protective effect Effects 0.000 description 8
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 8
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 7
- 238000006386 neutralization reaction Methods 0.000 description 7
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 7
- 229910001961 silver nitrate Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 238000005189 flocculation Methods 0.000 description 6
- 230000016615 flocculation Effects 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- 238000004846 x-ray emission Methods 0.000 description 6
- QGKMIGUHVLGJBR-UHFFFAOYSA-M (4z)-1-(3-methylbutyl)-4-[[1-(3-methylbutyl)quinolin-1-ium-4-yl]methylidene]quinoline;iodide Chemical compound [I-].C12=CC=CC=C2N(CCC(C)C)C=CC1=CC1=CC=[N+](CCC(C)C)C2=CC=CC=C12 QGKMIGUHVLGJBR-UHFFFAOYSA-M 0.000 description 5
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 5
- 229910021612 Silver iodide Inorganic materials 0.000 description 5
- 238000007792 addition Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- 229940045105 silver iodide Drugs 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 4
- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical compound [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 230000001235 sensitizing effect Effects 0.000 description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 description 4
- LRUDIIUSNGCQKF-UHFFFAOYSA-N 5-methyl-1H-benzotriazole Chemical compound C1=C(C)C=CC2=NNN=C21 LRUDIIUSNGCQKF-UHFFFAOYSA-N 0.000 description 3
- 238000001016 Ostwald ripening Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004133 Sodium thiosulphate Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 229940006461 iodide ion Drugs 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical class C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- GGZHVNZHFYCSEV-UHFFFAOYSA-N 1-Phenyl-5-mercaptotetrazole Chemical compound SC1=NN=NN1C1=CC=CC=C1 GGZHVNZHFYCSEV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000004285 Potassium sulphite Substances 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N alpha-ketodiacetal Natural products O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 2
- 229920006318 anionic polymer Polymers 0.000 description 2
- 150000001565 benzotriazoles Chemical class 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000007859 condensation product Substances 0.000 description 2
- 150000002334 glycols Chemical class 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- CMCWWLVWPDLCRM-UHFFFAOYSA-N phenidone Chemical compound N1C(=O)CCN1C1=CC=CC=C1 CMCWWLVWPDLCRM-UHFFFAOYSA-N 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 2
- 229940043349 potassium metabisulfite Drugs 0.000 description 2
- 235000010263 potassium metabisulphite Nutrition 0.000 description 2
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 2
- 235000019252 potassium sulphite Nutrition 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- LUMLZKVIXLWTCI-NSCUHMNNSA-N (e)-2,3-dichloro-4-oxobut-2-enoic acid Chemical compound OC(=O)C(\Cl)=C(/Cl)C=O LUMLZKVIXLWTCI-NSCUHMNNSA-N 0.000 description 1
- BCMCBBGGLRIHSE-UHFFFAOYSA-N 1,3-benzoxazole Chemical class C1=CC=C2OC=NC2=C1 BCMCBBGGLRIHSE-UHFFFAOYSA-N 0.000 description 1
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical class C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical class C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- YLVACWCCJCZITJ-UHFFFAOYSA-N 1,4-dioxane-2,3-diol Chemical compound OC1OCCOC1O YLVACWCCJCZITJ-UHFFFAOYSA-N 0.000 description 1
- KAMCBFNNGGVPPW-UHFFFAOYSA-N 1-(ethenylsulfonylmethoxymethylsulfonyl)ethene Chemical compound C=CS(=O)(=O)COCS(=O)(=O)C=C KAMCBFNNGGVPPW-UHFFFAOYSA-N 0.000 description 1
- IJHIIHORMWQZRQ-UHFFFAOYSA-N 1-(ethenylsulfonylmethylsulfonyl)ethene Chemical compound C=CS(=O)(=O)CS(=O)(=O)C=C IJHIIHORMWQZRQ-UHFFFAOYSA-N 0.000 description 1
- SIQZJFKTROUNPI-UHFFFAOYSA-N 1-(hydroxymethyl)-5,5-dimethylhydantoin Chemical compound CC1(C)N(CO)C(=O)NC1=O SIQZJFKTROUNPI-UHFFFAOYSA-N 0.000 description 1
- FYBFGAFWCBMEDG-UHFFFAOYSA-N 1-[3,5-di(prop-2-enoyl)-1,3,5-triazinan-1-yl]prop-2-en-1-one Chemical compound C=CC(=O)N1CN(C(=O)C=C)CN(C(=O)C=C)C1 FYBFGAFWCBMEDG-UHFFFAOYSA-N 0.000 description 1
- YGDWUQFZMXWDKE-UHFFFAOYSA-N 1-oxido-1,3-thiazole Chemical class [O-]S1=CN=C=C1 YGDWUQFZMXWDKE-UHFFFAOYSA-N 0.000 description 1
- JAAIPIWKKXCNOC-UHFFFAOYSA-N 1h-tetrazol-1-ium-5-thiolate Chemical class SC1=NN=NN1 JAAIPIWKKXCNOC-UHFFFAOYSA-N 0.000 description 1
- HAZJTCQWIDBCCE-UHFFFAOYSA-N 1h-triazine-6-thione Chemical class SC1=CC=NN=N1 HAZJTCQWIDBCCE-UHFFFAOYSA-N 0.000 description 1
- YKUDHBLDJYZZQS-UHFFFAOYSA-N 2,6-dichloro-1h-1,3,5-triazin-4-one Chemical compound OC1=NC(Cl)=NC(Cl)=N1 YKUDHBLDJYZZQS-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- BIEFDNUEROKZRA-UHFFFAOYSA-N 2-(2-phenylethenyl)aniline Chemical class NC1=CC=CC=C1C=CC1=CC=CC=C1 BIEFDNUEROKZRA-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- PHPYXVIHDRDPDI-UHFFFAOYSA-N 2-bromo-1h-benzimidazole Chemical class C1=CC=C2NC(Br)=NC2=C1 PHPYXVIHDRDPDI-UHFFFAOYSA-N 0.000 description 1
- AYPSHJCKSDNETA-UHFFFAOYSA-N 2-chloro-1h-benzimidazole Chemical class C1=CC=C2NC(Cl)=NC2=C1 AYPSHJCKSDNETA-UHFFFAOYSA-N 0.000 description 1
- KRTDQDCPEZRVGC-UHFFFAOYSA-N 2-nitro-1h-benzimidazole Chemical class C1=CC=C2NC([N+](=O)[O-])=NC2=C1 KRTDQDCPEZRVGC-UHFFFAOYSA-N 0.000 description 1
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical class OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N 2-propanol Substances CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- JSIAIROWMJGMQZ-UHFFFAOYSA-N 2h-triazol-4-amine Chemical class NC1=CNN=N1 JSIAIROWMJGMQZ-UHFFFAOYSA-N 0.000 description 1
- CBHTTYDJRXOHHL-UHFFFAOYSA-N 2h-triazolo[4,5-c]pyridazine Chemical class N1=NC=CC2=C1N=NN2 CBHTTYDJRXOHHL-UHFFFAOYSA-N 0.000 description 1
- OCVLSHAVSIYKLI-UHFFFAOYSA-N 3h-1,3-thiazole-2-thione Chemical class SC1=NC=CS1 OCVLSHAVSIYKLI-UHFFFAOYSA-N 0.000 description 1
- DSVIHYOAKPVFEH-UHFFFAOYSA-N 4-(hydroxymethyl)-4-methyl-1-phenylpyrazolidin-3-one Chemical compound N1C(=O)C(C)(CO)CN1C1=CC=CC=C1 DSVIHYOAKPVFEH-UHFFFAOYSA-N 0.000 description 1
- UTMDJGPRCLQPBT-UHFFFAOYSA-N 4-nitro-1h-1,2,3-benzotriazole Chemical class [O-][N+](=O)C1=CC=CC2=NNN=C12 UTMDJGPRCLQPBT-UHFFFAOYSA-N 0.000 description 1
- INVVMIXYILXINW-UHFFFAOYSA-N 5-methyl-1h-[1,2,4]triazolo[1,5-a]pyrimidin-7-one Chemical compound CC1=CC(=O)N2NC=NC2=N1 INVVMIXYILXINW-UHFFFAOYSA-N 0.000 description 1
- WSGURAYTCUVDQL-UHFFFAOYSA-N 5-nitro-1h-indazole Chemical compound [O-][N+](=O)C1=CC=C2NN=CC2=C1 WSGURAYTCUVDQL-UHFFFAOYSA-N 0.000 description 1
- GIQKIFWTIQDQMM-UHFFFAOYSA-N 5h-1,3-oxazole-2-thione Chemical compound S=C1OCC=N1 GIQKIFWTIQDQMM-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical class C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical class OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- XUYPXLNMDZIRQH-LURJTMIESA-N N-acetyl-L-methionine Chemical compound CSCC[C@@H](C(O)=O)NC(C)=O XUYPXLNMDZIRQH-LURJTMIESA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- YBGLHTDKCFKHTC-UHFFFAOYSA-L O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=S Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=S YBGLHTDKCFKHTC-UHFFFAOYSA-L 0.000 description 1
- ISLYUUGUJKSGDZ-UHFFFAOYSA-N OC1=CC=NC2=NC=NN12 Chemical class OC1=CC=NC2=NC=NN12 ISLYUUGUJKSGDZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- XEIPQVVAVOUIOP-UHFFFAOYSA-N [Au]=S Chemical compound [Au]=S XEIPQVVAVOUIOP-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000003926 acrylamides Chemical class 0.000 description 1
- 150000001253 acrylic acids Chemical class 0.000 description 1
- 150000008360 acrylonitriles Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000001346 alkyl aryl ethers Chemical class 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000002180 anti-stress Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- XHLMRAUSOZPJEM-UHFFFAOYSA-N benzenesulfonothioamide Chemical compound NS(=O)(=S)C1=CC=CC=C1 XHLMRAUSOZPJEM-UHFFFAOYSA-N 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical class C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 1
- 229960002303 citric acid monohydrate Drugs 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- QSAWQNUELGIYBC-UHFFFAOYSA-N cyclohexane-1,2-dicarboxylic acid Chemical compound OC(=O)C1CCCCC1C(O)=O QSAWQNUELGIYBC-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 150000004691 decahydrates Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- AFOSIXZFDONLBT-UHFFFAOYSA-N divinyl sulfone Chemical compound C=CS(=O)(=O)C=C AFOSIXZFDONLBT-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N ethyl formate Chemical compound CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 229940015043 glyoxal Drugs 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- AKCUHGBLDXXTOM-UHFFFAOYSA-N hydroxy-oxo-phenyl-sulfanylidene-$l^{6}-sulfane Chemical compound SS(=O)(=O)C1=CC=CC=C1 AKCUHGBLDXXTOM-UHFFFAOYSA-N 0.000 description 1
- WYASEAQTEQVOJE-UHFFFAOYSA-N hydroxy-phenyl-sulfanylidene-$l^{4}-sulfane Chemical compound OS(=S)C1=CC=CC=C1 WYASEAQTEQVOJE-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910001411 inorganic cation Inorganic materials 0.000 description 1
- 229910001505 inorganic iodide Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- CBEQRNSPHCCXSH-UHFFFAOYSA-N iodine monobromide Chemical compound IBr CBEQRNSPHCCXSH-UHFFFAOYSA-N 0.000 description 1
- 125000002346 iodo group Chemical group I* 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 244000145841 kine Species 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- ZAKLKBFCSHJIRI-UHFFFAOYSA-N mucochloric acid Natural products OC1OC(=O)C(Cl)=C1Cl ZAKLKBFCSHJIRI-UHFFFAOYSA-N 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 150000004957 nitroimidazoles Chemical class 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 150000004010 onium ions Chemical class 0.000 description 1
- 150000002924 oxiranes Chemical class 0.000 description 1
- QUBQYFYWUJJAAK-UHFFFAOYSA-N oxymethurea Chemical compound OCNC(=O)NCO QUBQYFYWUJJAAK-UHFFFAOYSA-N 0.000 description 1
- 229950005308 oxymethurea Drugs 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920013639 polyalphaolefin Polymers 0.000 description 1
- 229920006289 polycarbonate film Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229960003975 potassium Drugs 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 229960002816 potassium chloride Drugs 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- UGZVCHWAXABBHR-UHFFFAOYSA-O pyridin-1-ium-1-carboxamide Chemical class NC(=O)[N+]1=CC=CC=C1 UGZVCHWAXABBHR-UHFFFAOYSA-O 0.000 description 1
- HBCQSNAFLVXVAY-UHFFFAOYSA-N pyrimidine-2-thiol Chemical class SC1=NC=CC=N1 HBCQSNAFLVXVAY-UHFFFAOYSA-N 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000837 restrainer Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 235000017709 saponins Nutrition 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- JJJPTTANZGDADF-UHFFFAOYSA-N thiadiazole-4-thiol Chemical class SC1=CSN=N1 JJJPTTANZGDADF-UHFFFAOYSA-N 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 150000004684 trihydrates Chemical class 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
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
- G03C1/015—Apparatus or processes for the preparation of emulsions
-
- 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
- G03C5/16—X-ray, infrared, or ultraviolet ray processes
-
- 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
- G03C1/0051—Tabular grain emulsions
-
- 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
- G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
- G03C2001/03541—Cubic grains
-
- 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
- G03C2001/03558—Iodide content
-
- 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
- G03C2200/52—Rapid processing
Definitions
- the present invention relates to the preparation of silver halide emulsions, to X-ray silver halide photographic materials in which the said emulsions can be used and to the processing of said materials.
- Intrinsic sensitivity may be enhanced e.g. by enriching the iodide content of silver halide crystals to a certain extent. Moreover an enhanced amount of iodide will offer the possibility to get a better adsorption of certain spectral sensitizer.
- dye stain may become more important and the development may be inhibited as the lower solubility may make the kinetics of development and fixation decrease. This occurs in particular in rapid processing conditions due to the very short development, fixing and rinsing times which do not allow the total destruction and/or rinsing out of those sensitizing or non-sensitizing dyes.
- iodide ions have been built into the crystal volume and more particularly in the vicinity of and/or at the crystal surface is very critical to get a suitable compromise between high sensitivity (as a result of intrinsic sensitivity of the silver halide crystal and improved adsorption of spectral sensitizer) and rapid processability.
- a solution to provide a more homogenous micromixing has been found by the preparation of the initial nuclei in a reaction vessel that is smaller and separated from the bulk vessel as has e.g. been described in DE 1 472 745, DE 2 116 157 and DE 2 556 885, in US-Patents Nos. 3,705,034; 4,334,012; 4,336,328; 4,684,607 and 5,004,679 as well as in EP-Applications Nos. 326 852, 326 853, 370 116, 407 576, 355 535, 408 752, 368 275, 374 852, 374 853, 374 954.
- initial nuclei in a small separate reaction vessel is followed by growth of the said initial nuclei by means of further single or double jet precipation but also by means making use of the Ostwald ripening technique wherein the driving force for growing the silver halide crystals is the difference in crystal diameter between the initial nuclei and the added "feeding crystals" and/or the differences in solubility between both types of crystals.
- the initial crystals also called “nuclei”
- Ostwald ripening in the reaction vessel being separated from the vessel where the said nuclei are formed. Growth may occur by a difference in pAg between those two separated vessels, so that the dissolution step is fully determining the way in which silver iodide may be built in.
- a method for the preparation of a silver halide crystals comprising iodide in an amount of up to 3 mole % in the lattice of said crystals comprising the step of reacting a silver salt solution with a metal halide solution in the presence of at least one organic compound releasing iodide represented by the formula: A-L-I (I) wherein A represents a group with a positive Hammett ⁇ p value, commonly known as an electron-accepting or electon-withdrawing group, and L is a divalent linking group.
- a photographic material comprising a support and at least one silver halide emulsion layer on at least one side of said support coated from an emulsion containing silver iodohalide crystals prepared according to the method described hereinbefore.
- A is an electron-accepting or electron withdrawing, also called a group with a positive Hammett ⁇ p -Hammett value.
- Hammett ⁇ p values have been defined e.g. on p. 96 of "Structure/Activity Correlations for Drugs” published by Nankodo (1979).
- electron witdrawing groups are -COOH, -SO2R, -SO3R', etc. wherein R represents a substituted or unsubstituted aliphatic or aromatic group and R' represents an inorganic cation or an organic cationic group.
- a groups include a carboxylic acid group, a cyano group, a carbamoyl group, an acyl group, a sulphonyl group, an oxycarbonyl group, a sulphamoyl group.
- the organic compounds releasing iodide are preferably corresponding to the above formula wherein the divalent linking group is chosen from unsubstituted or substituted alkylene, unsubstituted or substituted oxyalkylene, unsubstituted or substituted aralkylene, or combinations of two or more thereof, wherein several atoms of L, or of A and L, can combine to form a ring, and wherein the iodine atom is not bound to an aromatic moiety or to an atom bearing a double bond, or to a hetero-atom.
- iodide ion slow releasers include following compounds : ICH2COOH (I-1) I(CH2)2COOH (I-2) I(CH2)3COOH (I-3) CH3CHICOOH (I-4) CH3CH2CHICOOH (I-5) CH3CHICH2COOH (I-6) HOOC-CHI-COOH (I-7) HOOC-CH2-CHI-COOH (I-8) ICH2CN (I-9) I(CH2)2CONH2 (I-10) ICH2COCH3 (I-11) I(CH2)2SO2CH3 (I-12) ICH2COOCH3 (I-13) ICH2CH2SO3Na (I-14) ICH2CONH2 (I-15) ICH2-CO-NH-C(CH2OH)3 (I-16) ICH2-CO-NH-C2H4-SO3Na (I-17) ICH2-CO-NH-CH2-(CHOH)4-CH2OH (I-18) In a particular preferred embodiment the following compounds ICH2
- the choice of a compound releasing iodide ions is mainly determined by its activity observed in real circumstances. E.g. the pH value of the medium and the presence of highly active nucleophilic ions have an important role therein.
- the iodide releaser is preferably used in aqueous solution in a concentration between 0.1 and 1 molar.
- a preferred compound present in the precipitation vessel is ammonia.
- the emulsions according to this invention can be prepared by the known methods like the single-jet method, wherein a iodohalide salt solution can be added to the solution containing a protective colloid in the reaction vessel before the start of the precipitation.
- a silver salt solution can be added during a predetermined time while stirring.
- Iodide ions may be distributed in a homogenous or heterogenous way over the silver iodohalide volume.
- a core-shell structure is typical for a crystal structure with a heterogenous distribution over its crystal volume.
- a (iodo)halide containing solution may consecutively be added to the reaction vessel after addition of a silver salt solution.
- This consecutive addition may be repeated in the presence of at least one organic compound releasing iodide in order to obtain different internal shell(s) containing silver iodide built up around the core.
- the core may be rich or poor in iodide ion concentration or may even be iodide free provided that at the start of the precipitation no iodide ions are present in the reaction vessel.
- the silver iodohalide crystals thus formed may have an outermost shell with a lower or a higher iodide concentration in comparison with an adjacent shell, depending on the precipitation conditions.
- the size distribution of the silver halide particles prepared according to this invention may be homodisperse or heterodisperse. Homodisperse distributions are obtained when 95 % of the grains have a size that does not deviate for more than 30 % from the average grain size. Average particle size diameters may vary over a wide range e.g. from 0.1 to 2.0 ⁇ m.
- the double-jet technique wherein a protective colloid solution is added to the reaction vessel before and wherein solutions of silver salts and halide salts are added simultaneously.
- the silver halide composition may be varied during the additions and especially when shells obtained by conversion with iodide ions are present, a combination of single and double jet precipitation techniques may be useful.
- said iodide ions are namely able to displace bromide and/or chloride ions from the grain, a technique known in the art as conversion.
- the said conversion step can also be performed at the silver halide crystal surface.
- a further precipitation technique may be the triple-jet technique to enhance the possibility to vary the halide composition in the volume of the crystals during precipitation. Combinations of single-jet, double-jet and triple-jet precipitation techniques are possible.
- iodide ions that are incorporated in the lattice of iodohalide crystals during precipitation are released from at least one organic compound releasing iodide ions. It may be useful to replace the said organic compound(s) partially by an inorganic iodide salt if required e.g. from kinetic considerations during precipitation.
- variable concentrations of solutions providing respectively silver and halide ions may be used during the different precipitation steps.
- Variable flow rates for the said solutions may be available during precipitation while controlling the pAg value and the temperature in the reaction vessel.
- the silver halide particles of the photographic emulsions according to the present invention may further have a regular crystalline form, e.g. cubic or octahedral or a transition form. Also an irregular crystalline form such as a spherical form or a tabular form may be obtained. Otherwise the emulsion crystals may have a composite crystal form comprising a mixture of said regular and irregular crystalline forms.
- the crystals may be doped with whatever a dope, as e.g. with Rh3+, Ir4+, Cd2+, Zn2+, Pb2+.
- the halide composition is chloroiodide, chlorobromoiodide or bromoiodide.
- the amount of iodide at certain sites within the crystal volume can vary between wide limits.
- cubic or tabular silver (chloro)bromoiodide or chloroiodide are preferred.
- chemical and/or spectral sensitizers can be added to the emulsion vessel. Further during precipitation grain growth restrainers or accelerators may be added.
- gelatin which is a thermoreversible polymer, showing a sufficient gel strength after coating.
- Conventional lime-treated or acid treated gelatin can be used. The preparation of such gelatin types has been described in e.g. "The Science and Technology of Gelatin", edited by A.G. Ward and A. Courts, Academic Press 1977, page 295 and next pages.
- the gelatin can also be an enzyme-treated gelatin as described in Bull. Soc. Sci. Phot. Japan, N° 16, page 30 (1966).
- Other types of protective colloids for use instead of or in addition to gelatin include various natural film-forming substances and synthetic resins, e.g.
- Coagulation in gelatineous medium can e.g. be effected by an alcohol or a salt or if the emulsion contains a sufficient amount of acid-coagulable gelatin derivatives or hydrogen bridge forming anionic polymeric compounds by addition of an acid to lower the pH value to the isoelectric point.
- Hydro bridge forming anionic polymeric compounds are polystyrene sulphonic acid and sulphonated copolymers of styrene, which are commonly used.
- Acid coagulable gelatin derivatives as phtaloyl or N-phenyl carbamoyl gelatin can be used, requiring only adjustment of the pH to the right value to cause the emulsion to coagulate.
- Suitable coagulation techniques have been described e.g. in U.S. Patent Specifications 2,614,928; 2,614,929 and 2,728,662.
- the silver halide emulsions can be precipitated in silica medium in the presence of a compound releasing iodide whereupon it is possible to apply the flocculation method as described in EP-A 517 961.
- Separately formed two or more different silver halide emulsions may be mixed for use in silver halide photographic materials in accordance with the present invention.
- the light-sensitive silver halide emulsion prepared according to the present invention can be chemically sensitized as described i.a. in the above-mentioned "Chimie et Physique Photographique” by P. Glafkides, in the above-mentioned “Photographic Emulsion Chemistry” by G.F. Duffin, in the above-mentioned “Making and Coating Photographic Emulsion” by V.L. Zelikman et al, and in "Die Grundlagen der Photographischen Sawe mit Silberhalogeniden” edited by H. Frieser and published by Akademische Verlagsgesellschaft (1968).
- chemical sensitization can be carried out by effecting the ripening in the presence of small amounts of compounds containing sulphur e.g. thiosulphate, thiocyanate, thioureas, sulphites, mercapto compounds, and rhodanines.
- sulphur e.g. thiosulphate, thiocyanate, thioureas, sulphites, mercapto compounds, and rhodanines.
- the emulsions can be sensitized also by means of gold-sulphur ripeners or by means of reductors e.g. tin compounds as described in GB-A 789,823, amines, hydrazine derivatives, formamidine-sulphinic acids, and silane compounds.
- Chemical sensitization can also be performed with small amounts of Ir, Rh, Ru, Pb, Cd, Hg, Tl, Pd, Pt, or Au.
- One of these chemical sensitization methods or a combination thereof can be used.
- a mixture can also be made of two or more separately precipitated emulsions being chemically sensitized before mixing them.
- spectral sensitizer(s) may be added to the redispersed silver halide emulsion. This may be performed with methine dyes such as those described by F.M. Hamer in "The Cyanine Dyes and Related Compounds", 1964, John Wiley & Sons. Dyes that can be used for the purpose of spectral sensitization include cyanine dyes, merocyanine dyes, complex cyanine dyes, complex merocyanine dyes, holopolar cyanine dyes, hemicyanine dyes, styryl dyes and hemioxonol dyes.
- Particularly valuable dyes are those belonging to the cyanine dyes, merocyanine dyes, complex merocyanine dyes.
- a survey of useful chemical classes of spectral sensitizing dyes and specific useful examples in connection with tabular grains is given in the already cited Research Disclosure Item 22534.
- Especially preferred green sensitizer in connection with the present invention are anhydro-5,5'-dichloro-3,3'-bis(n.sulfobutyl)-9-ethyloxacarbo-cyanine hydroxide and anhydro-5,5'-dichloro-3,3'-bis(n.sulfopropyl)-9-ethyloxacarbo-cyanine hydroxide.
- spectral sensitization In classical emulsion preparation spectral sensitization traditionally follows the completion of chemical sensitization. However, especially in connection with tabular grains having a large specific surface, it is specifically considered that spectral sensitization may occur simultaneously with or may even precede completely the chemical sensitization step: the chemical sensitization after spectral sensitization is believed to occur at one or more ordered discrete sites of tabular grains. This may also be done with emulsions, wherein the chemical sensitization proceeds in the presence of one or more phenidone and derivatives, a dihydroxy benzene as hydroquinone, resorcinol, catechol and/or a derivative(s) therefrom, one or more stabilizer(s) as e.g. 1-p-carboxyphenyl, 4,4' dimethyl-3-pyrazolidine-1-one, auxiliary agent(s) or antifoggant(s), one or more spectal sensitizer(s) or combinations of said ingredients
- Suitable supersensitizers are i.a. heterocyclic mercapto compounds containing at least one electronegative substituent as described e.g. in US-A 3,457,078, nitrogen-containing heterocyclic ring-substituted aminostilbene compounds as described e.g. in US-A 2,933,390 and US-A 3,635,721, aromatic organic acid/formaldehyde condensation products as described e.g. in US-A 3,743,510, cadmium salts, and azaindene compounds.
- To the silver halide emulsion prepared in accordance with the present invention may be added compounds preventing the formation of fog or stabilizing the photographic characteristics during the production or storage of photographic elements or during the photographic treatment thereof.
- Many known compounds can be added as fog-inhibiting agent or stabilizer to the silver halide emulsion. Suitable examples are i.a.
- heterocyclic nitrogen-containing compounds such as benzothiazolium salts, nitroimidazoles, nitrobenzimidazoles, chlorobenzimidazoles, bromobenzimidazoles, mercaptothiazoles, mercaptobenzothiazoles, mercaptobenzimidazoles, mercaptothiadiazoles, aminotriazoles, benzotriazoles (preferably 5-methyl-benzotriazole), nitrobenzotriazoles, mercaptotetrazoles, in particular 1-phenyl-5-mercapto-tetrazole, mercaptopyrimidines, mercaptotriazines, benzothiazoline-2-thione, oxazoline-thione, triazaindenes, tetrazaindenes and pentazaindenes, especially those described by Birr in Z.
- benzothiazolium salts such as benzothiazolium salts, nitroimidazoles, nitrobenzimidazoles, chlor
- the fog-inhibiting agents or stabilizers can be added to the silver halide emulsion prior to, during, or after the chemical ripening thereof and mixtures of two or more of these compounds can be used.
- the silver halide emulsions prepared in accordance with the present invention can be used to form one or more silver halide emulsion layers coated on a support to form a photographic silver halide element according to well known techniques.
- the photographic element of the present invention may comprise various kinds of surface-active agents in the photographic emulsion layer or in at least one other hydrophilic colloid layer.
- Suitable surface-active agents include non-ionic agents such as saponins, alkylene oxides e.g.
- polyethylene glycol polyethylene glycol/polypropylene glycol condensation products, polyethylene glycol alkyl ethers or polyethylene glycol alkylaryl ethers, polyethylene glycol esters, polyethylene glycol sorbitan esters, polyalkylene glycol alkylamines or alkylamides, silicone-polyethylene oxide adducts, glycidol derivatives, fatty acid esters of polyhydric alcohols and alkyl esters of saccharides; anionic agents comprising an acid group such as a carboxy, sulpho, phospho, sulphuric or phosphoric ester group; ampholytic agents such as aminoacids, aminoalkyl sulphonic acids, aminoalkyl sulphates or phosphates, alkyl betaines, and amine-N-oxides; and cationic agents such as alkylamine salts, aliphatic, aromatic, or heterocyclic quaternary ammonium salts, aliphatic or heterocyclic ring
- Such surface-active agents can be used for various purposes e.g. as coating aids, as compounds preventing electric charges, as compounds improving slidability, as compounds facilitating dispersive emulsification, as compounds preventing or reducing adhesion, and as compounds improving the photographic characteristics e.g higher contrast, sensitization, and development acceleration.
- Development acceleration can be accomplished with the aid of various compounds, preferably polyalkylene derivatives having a molecular weight of at least 400 such as those described in e.g. US-A 3,038,805 - 4,038,075 - 4,292,400.
- the photographic element of the present invention may further comprise various other additives such as e.g. compounds improving the dimensional stability of the photographic element, UV-absorbers, spacing agents, hardeners, and plasticizers as described below.
- additives such as e.g. compounds improving the dimensional stability of the photographic element, UV-absorbers, spacing agents, hardeners, and plasticizers as described below.
- the gelatin binder of the photographic elements can be forehardened with appropriate hardening agents such as those of the epoxide type, those of the ethylenimine type, those of the vinylsulfone type e.g. di-vinyl-sulphonyl-methane, ethylene di-(vinyl-sulphone), 1,3-vinylsulphonyl-2-propanol, bis-(vinylsulphonyl-methyl)-ether, chromium salts e.g. chromium acetate and chromium alum, aldehydes e.g. formaldehyde, glyoxal, and glutaraldehyde, N-methylol compounds e.g.
- appropriate hardening agents such as those of the epoxide type, those of the ethylenimine type, those of the vinylsulfone type e.g. di-vinyl-sulphonyl-methane, ethylene
- dimethylolurea and methyloldimethylhydantoin dioxan derivatives e.g. 2,3-dihydroxy-dioxan, active vinyl compounds as e.g. 1,3,5-triacryloyl-hexahydro-s-triazine, active halogen compounds e.g. 2,4-dichloro-6-hydroxy-s-triazine, and mucohalogenic acids e.g. mucochloric acid and mucophenoxychloric acid.
- These hardeners can be used alone or in combination.
- the binder can also be hardened with fast-reacting hardeners such as carbamoylpyridinium salts as disclosed in US Patent 4,063,952 and with the onium compounds as disclosed in EU Patent Application 408,143.
- the emulsion may be coated on any suitable substrate such as, preferably, a thermoplastic resin e.g. polyethyelenterephtalate or a polyethylene coated paper support.
- a thermoplastic resin e.g. polyethyelenterephtalate or a polyethylene coated paper support.
- suitable additives for improving the dimensional stability of the photographic element may be added, i.a. dispersions of a water-soluble or hardly soluble synthetic polymer e.g.
- Plasticizers suitable for incorporation in the emulsions according to the present invention are e.g. glycol, glycerine, or the latexes of neutral film forming polymers including polyvinylacetate, acrylates and methacrylates of lower alkanols, e.g. polyethylacrylate and polybutylmethacrylate.
- Suitable UV-absorbers are i.a. aryl-substituted benzotriazole compounds as described in US-A 3,533,794, 4-thiazolidone compounds as described in US-A 3,314,794 and 3,352,681, benzophenone compounds as described in JP-A 2784/71, cinnamic ester compounds as described in US-A 3,705,805 and 3,707,375, butadiene compounds as described in US-A 4,045,229, and benzoxazole compounds as described in US-A 3,700,455.
- the average particle size of spacing agents is comprised between 0.2 ⁇ m and 10 ⁇ m.
- Spacing agents can be soluble or insoluble in alkali. Alkali-insoluble spacing agents usually remain permanently in the photographic element, whereas alkali-soluble spacing agents usually are removed therefrom in an alkaline processing bath.
- Suitable spacing agents can be made i.a. of polymethyl methacrylate, of copolymers of acrylic acid and methyl methacrylate, and of hydroxypropylmethyl cellulose hexahydrophthalate. Other suitable spacing agents have been described in US-A 4,614,708.
- the photographic silver halide emulsions prepared according to the present invention can be used in various types of photographic elements such as i.a. in photographic elements for graphic arts and for so-called amateur and professional photography, diffusion transfer reversal photographic elements, low-speed and high-speed photographic elements, colour materials, X-ray materials, materials for micrographic applications etc..
- the said photographic silver halide emulsions are used in single side or double side coated X-ray materials.
- the photographic element with (an) emulsion(s) according to the present invention may contain one single emulsion layer, as it is the case for many applications, or it can be built up by two or even more emulsion layers.
- a material with a single or a duplitized emulsion layer coated on one or both sides of the support may contain silver halide emulsions according to this invention.
- duplitized emulsions differing in photographic speed by at least 0.15 log E a gain in cross-over in double side coated materials can be obtained.
- the material contains blue, green and red sensitive layers each of which can be single coated, but merely consist of double or even triple layers.
- the photographic material can contain several non-light sensitive layers, e.g. an antistress topcoat layer, one or more backing layers, and one or more intermediate layers eventually containing filter- or antihalation dyes that absorb scattering light and thus promote the image sharpness.
- Suitable light-absorbing dyes used in these intermediate layers are described in e.g. US Patents 4,092,168, US 4,311,787, DE 2,453,217, and GB Patent 7,907,440.
- One or more backing layers can be provided at the non-light sensitive side of the support of materials coated with at least one emulsion layer at only one side of the support.
- These layers which can serve as anti-curl layer can contain e.g. matting agents like silica particles, lubricants, antistatic agents, light absorbing dyes, opacifying agents, e.g. titanium oxide and the usual ingredients like hardeners and wetting agents.
- the support of the photographic material may be opaque or transparent, e.g. a paper support or resin support.
- a paper support preference is given to one coated at one or both sides with an Alpha-olefin polymer, e.g. a polyethylene layer which optionally contains an anti-halation dye or pigment.
- an organic resin support e.g. cellulose nitrate film, cellulose acetate film, poly(vinyl acetal) film, polystyrene film, poly(ethylene terephthalate) film, polycarbonate film, polyvinylchloride film or poly-Alpha-olefin films such as polyethylene or polypropylene film.
- the thickness of such organic resin film is preferably comprised between 0.07 and 0.35 mm.
- These organic resin supports are preferably coated with a subbing layer which can contain water insoluble particles such as silica or titanium dioxide.
- the photographic material with silver halide grains prepared according to the present invention can be image-wise exposed by any convenient radiation source in accordance with its specific application.
- processing conditions and composition of processing solutions are dependent from the specific type of photographic material in which the silver iodohalide grains prepared according to the present invention are applied.
- materials for X-ray diagnostic purposes said materials may be adapted to rapid processing conditions.
- an automatically operating processing apparatus is used provided with a system for automatic regeneration of the processing solutions.
- the forehardened material may be processed using one-part package chemistry or three-part package chemistry, depending on the processing application determining the degree of hardening required in said processing cycle.
- the developing and/or fixing step may proceed in hardener free processing solutions and replenishment of the developer and/or fixer solution may proceed by concentrate regeneration.
- reaction vessel 61.0 ml of solutions 1 and 2 were introduced into a reaction vessel in 28 seconds using the double jet technique.
- Said reaction vessel initially contained 2.16 liter of destilled water at 45°C, 12.6 grams of potassium bromide and 12.5 grams of gelatin. After one minute the reaction temperature of this mixture was raised to 70°C in 20 minutes and 47.5 grams of phthalated gelatin in 475 ml destilled water were added. After 10 minutes the neutralization step was started.
- a double jet precipitation was started using solutions 1 and 2 which continued for 40 minutes 51 seconds. During this precipitation, the pBr value was kept constant at 1.63. The flowing rate of solution 1 was 7.5 ml per minute at the start, linearly increasing to 22.2 ml per minute at the end of the precipitation. Thereafter the second neutralisation phaze was started.
- Second growth step (during which 62.0 mole % of the total amount of AgNO3 was used):
- This emulsion was prepared in the same way as comparative emulsion No. 1 with the only difference that after the second neutralization step 100 ml of solution 6 were added to the reaction vessel and that in the second growth step solution 7 was used instead of solution 3.
- This emulsion was prepared in the same way as inventive emulsion No. 1 with the only difference that after the second neutralization step 200 ml of solution 6 were added to the reaction vessel and that in the second growth step solution 8 was used instead of solution 7.
- This emulsion was prepared in the same way as inventive emulsion No. 1 with the only difference that after the second neutralization step 300 ml of solution 6 were added to the reaction vessel and that in the second growth step solution 9 was used instead of solution 7.
- Emulsions Nos. 1 to 3 were each optimally sulphur and gold sensitized in the presence of sodium thiocyanate and anhydro-5,5'-dichloro-3,3'-bis(n.sulfobutyl)-9-ethyloxacarbo-cyanine hydroxide in an amount of 660 mg per mole of silver nitrate.
- Each emulsion was stabilized with 4-hydroxy-6-methyl-1,3,3a,7-tetraazaindene and after addition of the normal coating additives the solutions were coated simultaneously together with a protective layer on both sides of a polyethylene terephthalate film support having a thickness of 175 ⁇ m.
- the resulting photographic material contained per side an amount of silver halide corresponding to 3.5 grams of AgNO3 per m2.
- the coating weight expressed in grams per square meter per side was 1.1 g of gelatin, 0.023 g of polymethylmethacrylate having a mean particle size of 3.5 ⁇ m and 0.1 g of formaldehyde as a hardening agent.
- CURIX HT530 (Agfa-Gevaert trademarked name) with the following time (in seconds) and temperature (in °C) characteristics: loading 0.2 sec. developing 9.3 sec. 35°C in developer I described below cross-over 1.4 sec. rinsing 0.9 sec. cross-over 1.5 sec. fixing 6.6 sec. 35°C in fixer I described below cross-over 2.0 sec. rinsing 4.4 sec. 20°C cross-over 4.6 sec. drying 6.7 sec. total 37.6 ⁇ sec.
- composition of the developer is composition of the developer:
- composition of the fixer ready-for-use is Composition of the fixer ready-for-use:
- Chemically sensitized fast monodisperse negative working silver bromoiodide emulsions having a varying iodide content were prepared in the following manner.
- the next 500 ml of silver nitrate were added at an increasing flow rate going from 15.5 ml/min. to 21.0 ml/min.
- the pAg was kept constant at the same value of 7.9 as for the core precipitation, but the halide composition was changed from a 100% KBr composition to a composition of 98 mole % KBr and 2 mole % KI for the shell. Over the whole silver bromoiodide crystal an average amount of 1 mole % of iodide ions was incorporated in this way.
- the redispersed emulsion was chemically sensitized for a period of 4 hours at 48°C in the presence of p-toluene thiosulphonate, sodium thiosulphate, sodium sulphite and a mixture of gold(III)-chloride and ammoniumthiocyanate so as to obtain an optimum in the relationship between fog and sensitivity.
- the emulsion was spectrally sensitized with anhydro-5,5'-dichloro-3,3'-bis(n.sulfobutyl)-9-ethyloxacarbo-cyanine hydroxide in an amount of 375 mg per mole of silver halide and stabilized with 4-hydroxy-6-methyl-1,3,3a-tetrazaindene before coating on a polyester support of 175 ⁇ m thickness.
- the emulsion layers were coated at a ratio of 6.8g/m2 of silver halide expressed as the equivalent amount of AgNO3.
- the whole precipitation, flocculation, redispersing and sensitization procedure was performed in the same way as for comparative emulsion No. 4, except for the presence instead of potassium iodide of monoiodoacetic acid in an equivalent amount as KI that was added so as to convert the silver bromide core after precipitation of 50 mole % of the total amount of silver nitrate.
- the whole precipitation, flocculation, redispersing and sensitization procedure was performed in the same way as for comparative emulsion No. 5, except for the presence instead of potassium iodide of monoiodoacetic acid in an equivalent amount as KI that was added so as to convert the silver bromide core after precipitation of 50 mole % of the total amount of silver nitrate.
- the emulsions were chemically sensitized for a period of 4 hours at 48°C in the presence of p-toluene thiosulphonate, sodium thiosulphate, sodium sulphite and of a mixture of gold(III)-chloride and ammoniumthiocyanate.
- the emulsions were spectrally sensitized with anhydro-5,5'-dichloro-3,3'-bis(n.sulfobutyl)-9-ethyloxacarbo-cyanine hydroxide in an, amount of 375 mg per mole of silver halide and stabilized with 4-hydroxy-6-methyl-1,3,3a-tetrazaindene before coating on a polyester support of 175 ⁇ m thickness.
- the emulsion layers were coated with silver halide crystals at a ratio of 6.8g/m2 of silver halide expressed as the equivalent amount of AgNO3.
- the photographic material samples were made by coating the emulsion on a polyethylene terephthalate support together with a composition for forming a protective gelatin layer.
- the amount of gelatin per square meter in the emulsion layers was 3.0 g, whereas in the protective layers it was 1.1 g.
- the developed photographic strips were fixed in a conventional fixing bath comprising e.g. sodium thiosulfate and potassium metabisulfite, and then rinsed in water and allowed to dry.
- a conventional fixing bath comprising e.g. sodium thiosulfate and potassium metabisulfite
- Sensitometric properties of these film strips are given in table III.
- This table shows the sensitometric results in terms of fog, sensitivity (log E(xposure)) and overall contrast of the photographic strips prepared and exposed as set forth above and developed in the developing bath of the composition set forth above during an overall developing time of 12 seconds.
- the gradation is measured from the characteristic curve over a density range of 1.75 starting from a density value of 0.25 to 2.00 above fog.
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP93203040A EP0651284A1 (de) | 1993-10-29 | 1993-10-29 | Fällung von Silberhalogenidkristallen, die lodid enthalten |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP93203040A EP0651284A1 (de) | 1993-10-29 | 1993-10-29 | Fällung von Silberhalogenidkristallen, die lodid enthalten |
Publications (1)
Publication Number | Publication Date |
---|---|
EP0651284A1 true EP0651284A1 (de) | 1995-05-03 |
Family
ID=8214150
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP93203040A Withdrawn EP0651284A1 (de) | 1993-10-29 | 1993-10-29 | Fällung von Silberhalogenidkristallen, die lodid enthalten |
Country Status (1)
Country | Link |
---|---|
EP (1) | EP0651284A1 (de) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0881530A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Emulsion von hohem Chloridgehalt hergestellt mittels Dimethylamine-Silberchlorojodid-Komplexverbindungen und Antischleiermittel |
EP0881531A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Herstellung einer Dimethylamin-Silberchlorjodid-Komplexverbindung und deren Verwendung als einzige Quelle für die Einbringung von Jodid in Silberchloridkristalle |
EP0881532A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Herstellung einer Dimethylamin-Silberbromojodid-Komplexverbindung und deren Verwendung als einzige Quelle für die Einbringung von Jodid in Silberbromidkristalle |
EP1150160A1 (de) * | 2000-04-25 | 2001-10-31 | Fuji Photo Film B.V. | Verfahren zur Herstellung einer photographischen Silberhalogenidemulsion |
US6630292B2 (en) | 2000-04-25 | 2003-10-07 | Fuji Photo Film B.V. | Method for producing a silver halide photographic emulsion |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0341728A2 (de) * | 1988-05-13 | 1989-11-15 | Fuji Photo Film Co., Ltd. | Photographische Silberhalogenidmaterialien |
EP0542354A1 (de) * | 1991-11-14 | 1993-05-19 | Agfa-Gevaert N.V. | Verfahren zum Entwickeln photographischer Röntgenmaterialien |
EP0561415A1 (de) * | 1992-03-19 | 1993-09-22 | Fuji Photo Film Co., Ltd. | Verfahren zur Herstellung einer photographischen Silberhalogenidemulsion, Emulsion und lichtempfindliches Material |
EP0563701A1 (de) * | 1992-03-19 | 1993-10-06 | Fuji Photo Film Co., Ltd. | Photographisches lichtempfindliches Silberhalogenidmaterial |
-
1993
- 1993-10-29 EP EP93203040A patent/EP0651284A1/de not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0341728A2 (de) * | 1988-05-13 | 1989-11-15 | Fuji Photo Film Co., Ltd. | Photographische Silberhalogenidmaterialien |
EP0542354A1 (de) * | 1991-11-14 | 1993-05-19 | Agfa-Gevaert N.V. | Verfahren zum Entwickeln photographischer Röntgenmaterialien |
EP0561415A1 (de) * | 1992-03-19 | 1993-09-22 | Fuji Photo Film Co., Ltd. | Verfahren zur Herstellung einer photographischen Silberhalogenidemulsion, Emulsion und lichtempfindliches Material |
EP0563701A1 (de) * | 1992-03-19 | 1993-10-06 | Fuji Photo Film Co., Ltd. | Photographisches lichtempfindliches Silberhalogenidmaterial |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0881530A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Emulsion von hohem Chloridgehalt hergestellt mittels Dimethylamine-Silberchlorojodid-Komplexverbindungen und Antischleiermittel |
EP0881531A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Herstellung einer Dimethylamin-Silberchlorjodid-Komplexverbindung und deren Verwendung als einzige Quelle für die Einbringung von Jodid in Silberchloridkristalle |
EP0881532A1 (de) * | 1997-05-30 | 1998-12-02 | Eastman Kodak Company | Herstellung einer Dimethylamin-Silberbromojodid-Komplexverbindung und deren Verwendung als einzige Quelle für die Einbringung von Jodid in Silberbromidkristalle |
EP1150160A1 (de) * | 2000-04-25 | 2001-10-31 | Fuji Photo Film B.V. | Verfahren zur Herstellung einer photographischen Silberhalogenidemulsion |
US6630292B2 (en) | 2000-04-25 | 2003-10-07 | Fuji Photo Film B.V. | Method for producing a silver halide photographic emulsion |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US5595864A (en) | Method for making tabular silver halide grains | |
EP0933670B1 (de) | Lichtempfindliche Emulsion mit bromidreichen Tafelkörnern, die mit Thiocyanatkomplexen des Rhodiums dotiert sind | |
EP0610609B1 (de) | Lichtempfindliches, photograhisches Silberhalogenidmaterial mit gesteigerter Bildqualität für Schnellverarbeitung zur Anwendung in der Mammographie | |
EP0528476B1 (de) | Verfahren zur Herstellung eines photographischen Silberhalogenidmaterials | |
EP0712034B1 (de) | Verfahren zur spektralen Sensibilisierung von tafelförmigen Silberhalogenidkörnern | |
EP0503700B1 (de) | Verfahren zur Herstellung von Jodobromid-Emulsionen, die monodisperse tabulare Körner enthalten | |
EP0677773A1 (de) | Tafelförmige Kristalle enthaltende Silberhalogenidemulsionen und Verfahren zu deren Verarbeitung | |
US6200743B1 (en) | Radiation-sensitive emulsion, light-sensitive silver halide photographic film material and radiographic intensifying screen-film combination | |
EP0651284A1 (de) | Fällung von Silberhalogenidkristallen, die lodid enthalten | |
EP0678772A1 (de) | Lichtempfindliches Silberchlorobromojodid- oder Silbuchlorojodid-Tafelkörner enthaltendes Material | |
EP0911687B1 (de) | Verfahren zur Herstellung von morphologisch homogenen silberbromidreichen tafelförmigen (111)-Kristallen | |
EP0569075B1 (de) | Verfahren zur Herstellung von tafelförmigen Silberhalogenid-Körnern | |
EP0653669B1 (de) | Chloridreiche Tafelkornemulsion mit (100)-Hauptflächen | |
US5733715A (en) | Silver halide photographic materials comprising silver bromide or bromoiodide emulsions having triangular tabular crystals | |
EP0770909A1 (de) | Photographisches Silberhalogenidmehrschichtmaterial und Verfahren zu dessen Herstellung | |
EP0610608B1 (de) | Photographisches, lichtempfindliches Silberhalogenidmaterial zur Wiedergabe von medizinischen laseraufgezeichneten Bildern und Verfahren zur Verarbeitung | |
EP0843208A1 (de) | Verfahren zur Herstellung silberbromidreicher Tafelkörner in Gegenwart spezifischer Gelatinen | |
US6436621B1 (en) | Multilayer silver halide photographic material and process for preparing the same | |
EP1045283B1 (de) | Strahlungsempfindliche Emulsion, lichtempfindlicher photographischer Silberhalogenidfilm und Kombination eines radiographischen Verstärkungsschirms mit einem Film | |
EP0634688B1 (de) | Spektral sensibilisierte photographische Materialien mit Tafelkörnern | |
US5795704A (en) | Method of hardener-free processing of a forehardened silver halide photographic material | |
EP0590715B1 (de) | Emulsionsherstellung mittels gleichzeitig durchgeführten chemischer und spektraler Sensibilisierung in Anwesenheit eines Salzes | |
EP0754964A1 (de) | Photographische Silberhalogenidmaterialien, die dreieckige Tafelkörner aufweisende Silberbromid- oder Bromidjodidemulsionen enthalten | |
US6080536A (en) | Method of preparing (100) tabular grains rich in silver bromide | |
US6312882B1 (en) | Silver halide emulsions comprising tabular crystals, emulsions and the processing thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): BE DE FR GB NL |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN |
|
18W | Application withdrawn |
Withdrawal date: 19960119 |