US3561262A - Water soluble developer - Google Patents
Water soluble developer Download PDFInfo
- Publication number
- US3561262A US3561262A US678176A US3561262DA US3561262A US 3561262 A US3561262 A US 3561262A US 678176 A US678176 A US 678176A US 3561262D A US3561262D A US 3561262DA US 3561262 A US3561262 A US 3561262A
- Authority
- US
- United States
- Prior art keywords
- water
- penetrant
- soluble
- developer
- film
- 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.)
- Expired - Lifetime
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 102
- 239000000126 substance Substances 0.000 abstract description 44
- 239000004094 surface-active agent Substances 0.000 abstract description 26
- 239000007788 liquid Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 20
- 239000007864 aqueous solution Substances 0.000 abstract description 19
- 238000012360 testing method Methods 0.000 abstract description 13
- 238000007689 inspection Methods 0.000 abstract description 11
- 238000001704 evaporation Methods 0.000 abstract description 10
- 230000008020 evaporation Effects 0.000 abstract description 10
- 239000003352 sequestering agent Substances 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 3
- 239000007850 fluorescent dye Substances 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 230000001464 adherent effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000003995 emulsifying agent Substances 0.000 abstract description 2
- 239000008233 hard water Substances 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical group [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 abstract 1
- 229920001296 polysiloxane Polymers 0.000 description 38
- 239000012530 fluid Substances 0.000 description 37
- 239000000203 mixture Substances 0.000 description 18
- 229920004929 Triton X-114 Polymers 0.000 description 16
- 239000000243 solution Substances 0.000 description 13
- 229920001223 polyethylene glycol Polymers 0.000 description 11
- 235000010234 sodium benzoate Nutrition 0.000 description 10
- 239000004299 sodium benzoate Substances 0.000 description 10
- 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 9
- 239000004202 carbamide Substances 0.000 description 9
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 8
- -1 Sodium nitrate Sodium bicarbonate Sodium carbonate Potassium nitrate Ammonium chloride Potassium iodide Sodium nitrite Chemical compound 0.000 description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 150000007524 organic acids Chemical class 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 239000000176 sodium gluconate Substances 0.000 description 6
- 235000012207 sodium gluconate Nutrition 0.000 description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 6
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 229940005574 sodium gluconate Drugs 0.000 description 5
- 239000001993 wax Substances 0.000 description 5
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 150000003863 ammonium salts Chemical class 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- IDOQDZANRZQBTP-UHFFFAOYSA-N 2-[2-(2,4,4-trimethylpentan-2-yl)phenoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=CC=C1OCCO IDOQDZANRZQBTP-UHFFFAOYSA-N 0.000 description 3
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229930006000 Sucrose Natural products 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000005985 organic acids Nutrition 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 235000010289 potassium nitrite Nutrition 0.000 description 3
- 239000004304 potassium nitrite Substances 0.000 description 3
- 235000010288 sodium nitrite Nutrition 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- KTUFKADDDORSSI-UHFFFAOYSA-N acebutolol hydrochloride Chemical compound Cl.CCCC(=O)NC1=CC=C(OCC(O)CNC(C)C)C(C(C)=O)=C1 KTUFKADDDORSSI-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical compound [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920000151 polyglycol Polymers 0.000 description 2
- 239000010695 polyglycol Substances 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229960004025 sodium salicylate Drugs 0.000 description 2
- MSXHSNHNTORCAW-GGLLEASOSA-M sodium;(2s,3s,4s,5r,6s)-3,4,5,6-tetrahydroxyoxane-2-carboxylate Chemical compound [Na+].O[C@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O MSXHSNHNTORCAW-GGLLEASOSA-M 0.000 description 2
- SDCULNUHRZODAC-UHFFFAOYSA-M sodium;2,5-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(C)C(S([O-])(=O)=O)=C1 SDCULNUHRZODAC-UHFFFAOYSA-M 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- 244000215068 Acacia senegal Species 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 241000416162 Astragalus gummifer Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 244000303965 Cyamopsis psoralioides Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007472 Leucaena leucocephala Species 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- 229920003091 Methocel™ Polymers 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- QPFYXYFORQJZEC-FOCLMDBBSA-N Phenazopyridine Chemical compound NC1=NC(N)=CC=C1\N=N\C1=CC=CC=C1 QPFYXYFORQJZEC-FOCLMDBBSA-N 0.000 description 1
- 241000920340 Pion Species 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical class C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 description 1
- 229920001615 Tragacanth Polymers 0.000 description 1
- YZBSTPDCHICUMO-UHFFFAOYSA-N [Cl-].C[NH+](C)C.C[NH+](C)C.CC1=C(C(=C(C=C1)C)C)CCCCCCCCCCCC.[Cl-] Chemical compound [Cl-].C[NH+](C)C.C[NH+](C)C.CC1=C(C(=C(C=C1)C)C)CCCCCCCCCCCC.[Cl-] YZBSTPDCHICUMO-UHFFFAOYSA-N 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003619 algicide Substances 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 1
- 150000008052 alkyl sulfonates Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- XKXHCNPAFAXVRZ-UHFFFAOYSA-N benzylazanium;chloride Chemical compound [Cl-].[NH3+]CC1=CC=CC=C1 XKXHCNPAFAXVRZ-UHFFFAOYSA-N 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- DPWCXHJKJXRDBZ-UHFFFAOYSA-N dec-5-yne-4,7-diol Chemical compound CCCC(O)C#CC(O)CCC DPWCXHJKJXRDBZ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical class CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 description 1
- SQEDZTDNVYVPQL-UHFFFAOYSA-N dodecylbenzene;sodium Chemical compound [Na].CCCCCCCCCCCCC1=CC=CC=C1 SQEDZTDNVYVPQL-UHFFFAOYSA-N 0.000 description 1
- 229960001484 edetic acid Drugs 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- FATAVLOOLIRUNA-UHFFFAOYSA-N formylmethyl Chemical group [CH2]C=O FATAVLOOLIRUNA-UHFFFAOYSA-N 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 125000000400 lauroyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000015250 liver sausages Nutrition 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920002113 octoxynol Polymers 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 229940070891 pyridium Drugs 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229960001790 sodium citrate Drugs 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- JWSRMCCRAJUMLX-UHFFFAOYSA-M sodium;4-aminonaphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(N)=CC=C(S([O-])(=O)=O)C2=C1 JWSRMCCRAJUMLX-UHFFFAOYSA-M 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- YFYABWXIJBTAAM-UHFFFAOYSA-M trimethyl(2-phenyltetradecan-2-yl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCC(C)([N+](C)(C)C)C1=CC=CC=C1 YFYABWXIJBTAAM-UHFFFAOYSA-M 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/91—Investigating the presence of flaws or contamination using penetration of dyes, e.g. fluorescent ink
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S252/00—Compositions
- Y10S252/96—Surface flaw detecting compositions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S516/00—Colloid systems and wetting agents; subcombinations thereof; processes of
- Y10S516/01—Wetting, emulsifying, dispersing, or stabilizing agents
Definitions
- 73104 12 Claims ABSTRACT OF THE DISCLOSURE A method for detecting flaws and other surface discontinuities by the liquid penetrant technique wherein an aqueous solution of a water soluble crystalline substance and a water dispersible surfactant serves as the developer for enhancing the visibility of flaw indications generated by the liquid penetrant.
- Said penetrant preferably contains a visible or fluorescent dye dissolved therein and is of an oily type which itself is not self emulsifying and is substantially free of any added emulsifying agent.
- the developer upon the evaporation or driving off of the water, forms an adherent film, or lattice layer, that is permeable to the liquid penetrant residue entrapped in any surface discontinuity so as to cause the penetrant residue to be drawn by capillarity or otherwise into said film and form therein flaw indications of high fidelity and resolution that may be easily detected upon inspection.
- the aqueous developer of this invention can optionally include film forming ingredients that effectively control the size of crystals formed upon drying; sequestering agents for use with hard water; and corrosion inhibiting agents; but the resulting film or lattice layer in all cases is entirely water soluble so that the surface of the test piece can be adequately cleaned by the use of water alone at the completion of the inspection step.
- the field of this invention is the art relating to the nondestructive method of detecting flaws and other surface discontinuities by the liquid penetrant technique.
- the De Forest et al. Patent No. 2,806,959 owned by the same assignee as the instant application, discloses the use of wet developers comprising suspensions of water-insoluble inorganic particles, such as talc, calcium carbonate, and the like in either an aqueous or an alcohol liquid suspending medium.
- the penetrant can be any of those described in the prior art, including the De Forest et al. Patent No. 2,806,959, but our invention is particularly applicable to the penetrant method in which the liquid penetrant is a water immiscible oil. such as a petroleum hydrocarbon, and contains either a visible or a fluorescent dye dissolved therein.
- an aqueous solution is prepared for use as a developer by dissolving in water a water-soluble crystalline substance and dispersing therein a surfactant that is compatible with the crystalline substance upon crystallization thereof by the evaporation of water from the solution to deposit upon the surface of the test piece a water-soluble film permeable by the penetrant residue to give it a flaw indication of enhanced visibility in the inspection thereof.
- the term water-soluble is a relative term, the use of the term herein will be understood to represent a degree of solubility far in excess of that of the pigments that have heretofore been used in wet developers.
- the crystalline substances used in the present aqueous solution type developer have a solubility of at least 1 gram in 100 cc. of water at 20 C., and are used in our aqueous solution type developer in a concentration of at least one-half percent by weight up to saturation and even super-saturation concentrations.
- the surfactant used with the crystalline substance need not be completely in solution in the developer in the state in which it is used, since some surfactants useful for our purpose give slightly cloudy or even turbid properties to the resulting aqueous solution type developer, but in all cases the surfactant used is one that is compatible with the crystalline substance employed to give, upon evaporation of the water content, a dry deposit that is completely water-soluble. Accordingly, the residue of the dry-deposit formed on the surface of the test piece can be completely removed by washing with water alone, after the inspection step has been completed, so as to leave a clean surface.
- the aqueous solution developer consists essentially of a watersoluble crystalline substance, which may be either inorganic, organic or metallo-organic, provided it is soluble at least to the extent of one percent by weight; a water dispersible surfactant within the range of from 0.1 to 5% by weight of the solution, which is compatible with the crystalline substance within the definition above given; and optionally a water-soluble film-forming substance within the range of from 0l0%, a water-soluble sequestering agent between the range of from 0 to 5%, a water-soluble corrosion inhibitor within the range of 0 to 5%, and the balance, water.
- a watersoluble crystalline substance which may be either inorganic, organic or metallo-organic, provided it is soluble at least to the extent of one percent by weight
- a water dispersible surfactant within the range of from 0.1 to 5% by weight of the solution, which is compatible with the crystalline substance within the definition above given
- optionally a water-soluble film-forming substance within the
- Trito Xl 14 is just one example of the many surfactants which could be used. Any Water-soluble surfactant stable in the electrolyte medium employed is satisfactory for use. Where sulfur and chlorine content are of concern (because of presenting embrittlement problems) it is desirable to employ surfactants which are free of sulfur and chlorine.
- L-77 silicone fluid is a super wetter," and can be used alone, as the surfactant. It is a proprietary product of Union Carbide Corporation, along with other organo silicone surfactants, and is believed to be the reaction product of an organic silicone (siloxane) and a nonionic wetting agent. It is only very slightly soluble in water.
- any of the water soluble crystalline inorganic substances previously listed can be used within the ranges of percentages and in the percentages by weight shown for those in the following:
- EXAMPLE 10 Percent Water soluble inorganic substance (to saturation) 1 Surfactant 0.1 to 5 Water Balance EXAMPLE ll, WITH CORROSION INHIBITOR Percent Potassium nitrite l0 Triton X114 l L-77 silicone fluid 0.1 Sodium nitrite 5 Sodium dichromate 0.4 Water 88.5
- Sodium dichromate protects aluminum from corroding, but does alter to a degree the fluorescense of the indications.
- tetra sodium pyrophosphate can be used and in the same amount.
- sodium salicylate, sodium citrate, potassium citrate, ammonium acetate, sodium gluconate and other water soluble metal or ammonium salts of organic acids can be satisfactorily used in various proportions depending upon their solubilities within the broad limits given herein.
- EXAMPLE 20 Percent Water soluble metal or NH salt of an organic acid (to saturation) 0.5 Surfactant 0.1 to 5 Film former 0 to 10 Water Balance EXAMPLE 21, SPECIFIC MIXTURE Percent Sodium benzoate 10 Sodium gluconate 1 Triton X1l4 1 L77 silicone fluid 0.1 Water 87.9
- surfactants that have been found satisfactory for use in our aqueous solution type developer composition are the following, but in general any surfactant, whether nonionic, cationic or anionic, that is water dispersible, has good wetting properties and is compatible with the other ingredients of the composition to form a completely Water soluble film or lattice deposit, when dried, can be used alone or in combination:
- Neodol 25-9-Shell Refining Company (2) Neodol 23-6 /zShel] Refining Company (3) Biosoft EA Series-Stepan Chemical Company (B) Alkylphenol polyglycol ethers:
- Triton X Seriesisooctyl phenyl polyethoxyethanolsX-l00, Xl02, X1l4Rohm 8L Haas Triton N Seriesnonyl phenyl polyoxyethanols NllRohm & Haas (3) Surfonic N Seriesalkylaryl polyethylene glycol ethersN-60, N-95, N-200, N300Jefferson Chemical Company (4) lgepal CO Seriesnonylphenoxy poly (ethyleneoxy) ethanolGeneral Aniline & Film Company (5) Stepanol B-l29sodium salt of an alkylphenoxy poly oxyethyleneStepan Chemical Comp y (C) Fatty acid esters of polyglycol ethers:
- the preferred water soluble developer composition of our invention in its dry form, has the following formula, expressed in percentages by weight:
- Carbowax 4000 is a proprietary synthetic, Water-soluble wax having a water solubility of 100 grams per 100 cc.
- EDTA is the abbreviation for ethylene diamine tetraacetic acid.
- Other sequestering agents such as those previously named herein can be employed, especially sodium D-gluconate.
- L77 silicone fluid has outstanding wetting and spreading characteristics and can be used by itself at extremely low concentrations (0.05 to 0.10%) by weight of the aqueous solution of the selected crystalline substance or mixture of crystalline substances.
- Other surfactants such as those already listed herein, can be used in the same percentage as given in Example 35 or Within the broad range of percentages herein given.
- the surfactant, as well as the other components of our developer composition should be substantially or wholly free of sulfur and chlorine.
- Hyamin 2389 which is water soluble, non-toxic and functions as a cationic wetting agent. It functions particularly well with L77 silicon fluid.
- Hyamin 2389 is a mixture of methyl-dodecylbenzyl-trimethyl ammonium chloride, 10% methyldodecylxylene bis-trimethyl ammonium chloride as a aqueous solution, and can be used in concentrations of from 10 to 400 ppm.
- the dry composition e.g. that of Example 35, can be diluted with or dissolved in water to any extent within the broad ranges of percent by weight given in the following example:
- a workable concentration of the crystalline substance is obtained by using from A lb. of the dry composition per gallon up to as high as saturation, 3 lbs/gal. of water or even higher.
- An average solution concentration is 1 lb. of the dry composition per gal. of water.
- aqueous solution consisting essentially of a water-soluble crystalline substance present in an amount of at least 0.5% by weight up to saturation
- a water dispersible surfactant compatible with said water-soluble crystalline substance and present in an amount from 0.1% to 10% by weight of said solution; said water dispersible surfactant being compatible with said water-soluble crystalline substance upon crystallization of the latter by evaporation of Water from said solution to deposit on said test piece surface a water soluble crystalline film permeable by said penetrant residue to give a flaw indication of enhanced visibility upon inspection thereof.
- said liquid penetrant is an oil
- said surfactant is miscible with said oil to effect migration of said penetrant residue into said water soluble film.
- water-soluble crystalline substance from 0.5% to saturation.
- water-soluble surfactant from 0.1% to 5%, water-soluble film-forming substance from to 10%
- water-soluble sequestering agent from 0 to water-soluble corrosion inhibitor from 0 to 5 and the balance water, said solution upon evaporation leaving a penetrant permeable crystalline film removable by water washing alone.
- said water-soluble crystalline substance is sodium benzoate
- said water-soluble film-forming substance is a normally solid, non-volatile water-soluble wax having a water solubility of 100 grams per 100 cc. at 20 C.
- An aqueous solution for use as a water-soluble developer in the liquid penetrant method of detecting surface discontinuities in a test piece consisting essentially of the following:
- a water-soluble developer for use in the liquid penetrant method of detecting surface discontinuities in a test piece comprising an aqueous solution consisting essentially of the following:
- a water-soluble film-forming, normally water-soluble wax in an amount up to 10% and sufficient to produce uniformly sized small crystals of said sodium benzoate, from 0 to 5% of a corrosion inhibitor, and the balance being largely water, said solution upon evaporation of the water leaving a water-soluble crystalline film permeable by the liquid penetrant to form a fiaw indication of enhanced visibility upon inspection.
- An aqueous solution for use as a water-soluble developer in the liquid penetrant method of detecting surface discontinuities in the test piece consisting essentially 0 of the following:
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Abstract
A METHOD FOR DETECTING FLAWS AND OTHER SURFACE DISCONTINUTIES BY THE LIQUID PENETRANT TECHNIQUE WHEREIN AN AQUEOUS SOLUTION OF A WATER SOLUBLE CRYSTALLINE SUBSTANCE AND A WATER DISPERSIBLE SURFACTANT SERVES AS THE DEVELOPER FOR ENCHANCING THE VISIBILITY OF FLAW INDICATIONS GENERATED BY THE LIQUID PENETRANT. SAID PENETRANT PREFERABLY CONTAINS A VISIBLE OR FLUORESCENT DYE DISSOLVED THEREIN AND IS OF AN OILY TYPE WHICH ITSELF IS NOT SELFEMULSIFYINGT AND IS SUBSTANTIALLY FREE OF ANY ADDED EMULSIFYING AGENT. THE DEVELOPER, UPON THE EVAPORATION OR DRIVING OFF OF THE WATER, FORMS AN ADHERENT FIL, OR LATTICE LAYER, THAT IS PERMEABLE TO THE LIUQID PENETRANT RESIDUE ENTRAPPED IN ANY SURFACE DISCONTAINUITY SO AS TO CAUSE THE PENETRANT RESIDUE TO BE DRAWN BY CAPILLARITY OR OTHERWISE INTO SAID FILM AND FORM THEREIN FLAW INDICATIONS OF HIGH FIDELITY AND RESOLUTION THAT MAY BE EASILY DETECTED UPON INSPECTION. THE AQUEOUS DEVELOPER OF THIS INVENTION CAN OPTIONALLY INCLUDE FILM FORMING INGREDIENTS THAT EFFECTIVELY CONTROL THE SIZE OF CRYSTALS FORMED UPON DRYING; SEQUESTERING AGENTS FOR USE WITH HARD WATER; AND CORROSION INHIBITING AGENTS; BUT THE RESULTING FILM OR LATTICE LAYER IN ALL CASES IS ENTIRELY WATER SOLUBLE SO THAT THE SURFACE OF THE TEST PIECE CAN BE ADEQUATELY CLEANED BY THE USE OF WATER ALONE AT THE COMPLETION OF THE INSEPCTION STEP.
Description
United States Patent Office 3,561,262 Patented Feb. 9, 1971 3,561,262 WATER SOLUBLE DEVELOPER James S. Borucki, Chicago, and Bruce C. Graham, Arlington Heights, 111., assignors to Magnaflux Corporation, Chicago, Ill., a corporation of Delaware No Drawing. Filed Oct. 26, 1967, Ser. No. 678,176 Int. Cl. Gllln 19/08 US. Cl. 73104 12 Claims ABSTRACT OF THE DISCLOSURE A method for detecting flaws and other surface discontinuities by the liquid penetrant technique wherein an aqueous solution of a water soluble crystalline substance and a water dispersible surfactant serves as the developer for enhancing the visibility of flaw indications generated by the liquid penetrant. Said penetrant preferably contains a visible or fluorescent dye dissolved therein and is of an oily type which itself is not self emulsifying and is substantially free of any added emulsifying agent. The developer, upon the evaporation or driving off of the water, forms an adherent film, or lattice layer, that is permeable to the liquid penetrant residue entrapped in any surface discontinuity so as to cause the penetrant residue to be drawn by capillarity or otherwise into said film and form therein flaw indications of high fidelity and resolution that may be easily detected upon inspection. The aqueous developer of this invention can optionally include film forming ingredients that effectively control the size of crystals formed upon drying; sequestering agents for use with hard water; and corrosion inhibiting agents; but the resulting film or lattice layer in all cases is entirely water soluble so that the surface of the test piece can be adequately cleaned by the use of water alone at the completion of the inspection step.
CROSS-REFERENCE TO RELATED APPLICATION pigmented developer, whether the liquid is water or an organic solvent, the pigment left behind on the surface of the test piece after development and inspection of any flaw indication is very diflicult to remove and cannot be effectively and completely removed by a stream of water alone, as is true of the water-soluble residue left on the surface of the work piece upon evaporation of the water from the present aqueous solution-type developer.
BACKGROUND OF THE INVENTION The field of this invention is the art relating to the nondestructive method of detecting flaws and other surface discontinuities by the liquid penetrant technique. The De Forest et al. Patent No. 2,806,959, owned by the same assignee as the instant application, discloses the use of wet developers comprising suspensions of water-insoluble inorganic particles, such as talc, calcium carbonate, and the like in either an aqueous or an alcohol liquid suspending medium. Since the water-insoluble pigment of the prior art liquid type developers was relied upon to function as the developer by reason of its blotting effect upon the liquid penetrant entrapped in any flaws in the test piece surface, the total omission of any such pigments from the aqueous solution developer of the present invention is clearly an unobvious departure from what was heretofore known by workers in this art.
SUMMARY OF THE INVENTION In the liquid penetrant technique, to which this invention relates, the penetrant can be any of those described in the prior art, including the De Forest et al. Patent No. 2,806,959, but our invention is particularly applicable to the penetrant method in which the liquid penetrant is a water immiscible oil. such as a petroleum hydrocarbon, and contains either a visible or a fluorescent dye dissolved therein.
In accordance with the prent invention, an aqueous solution is prepared for use as a developer by dissolving in water a water-soluble crystalline substance and dispersing therein a surfactant that is compatible with the crystalline substance upon crystallization thereof by the evaporation of water from the solution to deposit upon the surface of the test piece a water-soluble film permeable by the penetrant residue to give it a flaw indication of enhanced visibility in the inspection thereof.
Since the term water-soluble" is a relative term, the use of the term herein will be understood to represent a degree of solubility far in excess of that of the pigments that have heretofore been used in wet developers. In contrast to such pigments as calcium carbonate, talc, and silica, having a water-solubility in general less than about 0.001 gram in 100 cc. of water, the crystalline substances used in the present aqueous solution type developer have a solubility of at least 1 gram in 100 cc. of water at 20 C., and are used in our aqueous solution type developer in a concentration of at least one-half percent by weight up to saturation and even super-saturation concentrations.
The surfactant used with the crystalline substance need not be completely in solution in the developer in the state in which it is used, since some surfactants useful for our purpose give slightly cloudy or even turbid properties to the resulting aqueous solution type developer, but in all cases the surfactant used is one that is compatible with the crystalline substance employed to give, upon evaporation of the water content, a dry deposit that is completely water-soluble. Accordingly, the residue of the dry-deposit formed on the surface of the test piece can be completely removed by washing with water alone, after the inspection step has been completed, so as to leave a clean surface.
In the broadest embodiment of our invention, the aqueous solution developer consists essentially of a watersoluble crystalline substance, which may be either inorganic, organic or metallo-organic, provided it is soluble at least to the extent of one percent by weight; a water dispersible surfactant within the range of from 0.1 to 5% by weight of the solution, which is compatible with the crystalline substance within the definition above given; and optionally a water-soluble film-forming substance within the range of from 0l0%, a water-soluble sequestering agent between the range of from 0 to 5%, a water-soluble corrosion inhibitor within the range of 0 to 5%, and the balance, water.
The following are some of the water-soluble crystalline substances that can be used in our aqueous solution type developer:
Inorganic solubles Sodium nitrate Sodium bicarbonate Sodium carbonate Potassium nitrate Ammonium chloride Potassium iodide Sodium nitrite Inorganic solubles Aluminum chloride Potassium chloride Sodium chloride Organic compounds Urea Sucrose Resorcinol Ethylene diamine tetramine acetic acid, sodium salt Metallo-organic salts Sodium citrate Potassium citrate Ammonium acetate Sodium gluconate Sodium benzoate Sodium salicylate The following are compositions expressed in percentages by weight, of our aqueous solution type developers:
(I) Based upon the use of inorganic crystalline substances:
EXAMPLE 1 Percent Ammonium chloride 10 Triton X114 I L-77 silicone fluid 0.1 Water 88.9
EXAMPLE 2 Percent Potassium nitrate 10 Triton X114 1 L-77 silicone fluid 0.1 Water 88.9
EXAMPLE 3 Percent Sodium bicarbonate 3 Triton X114 1 L-77 silicone fluid 0.1 Water 95.9
EXAMPLE 4 Percent Sodium carbonate 3 Triton X-l14 1 L-77 silicone fluid 0.1 Water 95.9
EXAMPLE 5 Percent Potassium iodide 10 Triton X114 1 L-77 silicone fluid 0.1 Water 88.9
EXAMPLE 6 Percent Sodium nitrite 10 Triton X114 1 L-77 silicone fluid 0.1 Water 88.9
EXAMPLE 7 Percent Aluminum chloride I0 Triton X114 I L-77 silicone fluid 0.1 Water 88.9
EXAMPLE 8 Percent Sodium chloride 10 Triton X114 1 L-77 silicone fluid 0.1 Water 88.9
4 EXAMPLE 9 Percent Potassium chloride 10 Triton X114 l L-77 silicone fluid 0.1 Water 88.9
Trito Xl 14 is just one example of the many surfactants which could be used. Any Water-soluble surfactant stable in the electrolyte medium employed is satisfactory for use. Where sulfur and chlorine content are of concern (because of presenting embrittlement problems) it is desirable to employ surfactants which are free of sulfur and chlorine.
L-77 silicone fluid is a super wetter," and can be used alone, as the surfactant. It is a proprietary product of Union Carbide Corporation, along with other organo silicone surfactants, and is believed to be the reaction product of an organic silicone (siloxane) and a nonionic wetting agent. It is only very slightly soluble in water.
Any of the water soluble crystalline inorganic substances previously listed can be used within the ranges of percentages and in the percentages by weight shown for those in the following:
EXAMPLE 10 Percent Water soluble inorganic substance (to saturation) 1 Surfactant 0.1 to 5 Water Balance EXAMPLE ll, WITH CORROSION INHIBITOR Percent Potassium nitrite l0 Triton X114 l L-77 silicone fluid 0.1 Sodium nitrite 5 Sodium dichromate 0.4 Water 88.5
EXAMPLE 12, WITH SEQUESTERING AGENT Percent Potassium nitrite 10 Triton X114 1 L-77 silicone fluid 0.1 Sodium gluconate 1 Water 87.9
Sodium dichromate protects aluminum from corroding, but does alter to a degree the fluorescense of the indications. In formulations where this is a problem, tetra sodium pyrophosphate can be used and in the same amount.
Other sequestering agents than sodium gluconate can be used.
Examples:
(1) EDTA (2) Versene series (3) Questol series EXAMPLE 13, WITH MIXED WATER SOLUBLE CRYSTALLINE INORGANIC SUBSTANCES Percent Potassium nitrite 10 Sodium bicarbonate 3 Triton X114 1 L-77 silicone fluid 0.1 Water 85.9 EXAMPLE 14, WITH CARBOWAX AS THE FILM FORMER Percent Ammonium chloride 10 Triton X114 l L-77 silicone fluid 0.1 Carbowax 4000 5 Water 83.9
EXAMPLE 15 Percent Sodium bicarbonate 3 Triton X-114 1 L77 silicone fluid 0.1 Carbowax 4000 5 Water 90.9
EXAMPLE 16 Percent Sodium borate 1 Triton X-1l4 1 L77 silicone fluid 0.1 Water 97.9
(II) Based upon the use of water soluble metal or ammonium salts of organic acids:
EXAMPLE 17 Percent Sodium benzoate Triton X-114 1 L77 silicone fluid 0.1 Water 88.9
In place of sodium benzoate in Example 17, sodium salicylate, sodium citrate, potassium citrate, ammonium acetate, sodium gluconate and other water soluble metal or ammonium salts of organic acids can be satisfactorily used in various proportions depending upon their solubilities within the broad limits given herein.
EXAMPLE 18 Percent 2,5 dimethylbenzenesulfonic acid sodium salt 2 Triton X-114 l L77 silicone fluid 0.1 Water 96.9
EXAMPLE 19 Percent 4-amino naphthalenesulfonic acid sodium salt 2 Triton X114 1 L77 silicone fluid 0.1 Water 96.9
Any of the water soluble metal or ammonium salts of organic acids previously listed can be used within the ranges of and in the percentages by weight given in the following:
EXAMPLE 20 Percent Water soluble metal or NH salt of an organic acid (to saturation) 0.5 Surfactant 0.1 to 5 Film former 0 to 10 Water Balance EXAMPLE 21, SPECIFIC MIXTURE Percent Sodium benzoate 10 Sodium gluconate 1 Triton X1l4 1 L77 silicone fluid 0.1 Water 87.9
EXAMPLE 22, SPECIFIC Percent Sodium benzoate 10 Carbowax 4000 2 Triton X-l14 1 L77 silicone fluid 0.1 Water 86.9
EXAMPLE 23 Percent 2,5 dimethylbenzenesulfonic acid sodium salt 2 CarboWax 4000 2 Triton X-1l4 1 L77 silicone fluid 0.1 Water 94.9
(III) Based upon the use of water soluble organic compounds:
EXAMPLE 24 Percent Urea 10 L77 silicone fluid (l.l
Water 89.l
EXAMPLE 25 Percent Sucrose 10 L77 silicone fluid 0.1
Water 89.l
EXAMPLE 26 Percent Resorcinol 5 L77 silicone fluid 0.1
Water 94.9
EXAMPLE 27 Percent 2 butyne 1,4 diol 5 L77 silicone fluid 0.1
Water 94.9
EXAMPLE 28 Percent Acetamide 5 L77 silicone fluid 0.1
Water 94.9
EXAMPLE 29 Hydrazine sulfate l L77 silicone fluid 0.1
Water 98.9
(IV) Based upon the use of a blend of water soluble organic compounds:
EXAMPLE 30 Percent Urea 5 Sucrose 5 L77 silicone fluid 0.l Water 89.9
EXAMPLE 31 Percent Urea 6 Resorcinol 4 L77 silicone fluid 0.1 Water 89.9
(V) Based upon the use of a blend of water soluble organic compounds and inorganic salts:
EXAMPLE 32 Percent Urea 8 Sodium bicarbonate 2 L77 silicone fluid 0.1 Water 89.9
EXAMPLE 33 Percent Urea 8 Sodium nitrite 2 L77 silicone fluid 0.1 Water 89.9
EXAMPLE 34 Percent Urea 5 Potassium nitrate S L77 silicone fluid 0.1 Water 89.9
Surfactants that have been found satisfactory for use in our aqueous solution type developer composition are the following, but in general any surfactant, whether nonionic, cationic or anionic, that is water dispersible, has good wetting properties and is compatible with the other ingredients of the composition to form a completely Water soluble film or lattice deposit, when dried, can be used alone or in combination:
(I) Non-ionic:
(A) Ethoxy fatty alcohols:
(1) Neodol 25-9-Shell Refining Company (2) Neodol 23-6 /zShel] Refining Company (3) Biosoft EA Series-Stepan Chemical Company (B) Alkylphenol polyglycol ethers:
(1) Triton X Seriesisooctyl phenyl polyethoxyethanolsX-l00, Xl02, X1l4Rohm 8L Haas (2) Triton N Seriesnonyl phenyl polyoxyethanols NllRohm & Haas (3) Surfonic N Seriesalkylaryl polyethylene glycol ethersN-60, N-95, N-200, N300Jefferson Chemical Company (4) lgepal CO Seriesnonylphenoxy poly (ethyleneoxy) ethanolGeneral Aniline & Film Company (5) Stepanol B-l29sodium salt of an alkylphenoxy poly oxyethyleneStepan Chemical Comp y (C) Fatty acid esters of polyglycol ethers:
(l) Stepanol TBI(an alkoxypolyoxyethylene ethanolStepan Chemical Company (D) Alkanolamides:
(1) Sole Terge 325-lauric alkanolaminesHod-ag Chemical (2) Sole Terge 59K--mixed fatty alkanolamines Hodag Chemical Company (3) Ninol l281mixed fatty alkanolamines-Stepan Chemical Company (4) Ninol l285fatty acid alkanolamines--Stepan Chemical Company (E) Acetylenic glycols and their ethoxylated derivatives:
(1) Surfynol l04acetylenic glycol 2, 4, 7, 9 tetramethylAirco Chemical (2) Surfynol T.G.a mixture of 5-decyne-4.7 diol. 100% concentration of 104, and an alkylphenyl ether of polyethylene glycol in ethylene glycol surfynol, 83% concentration (F) Ethoxylated fatty acid esters of sorbitan (G) L-77 silicone fluid non-ionic wetting agent-Union Carbide (II) Cationic:
(A) Alkyl aryl quatenary ammonium salts:
(l) Katapone VV328an alkyl polyethoxyethanol benzylammonium chloride, 85% concentration General Aniline & Film Corporation (2) Hyamine 3500N-alkyl (C C C dimethylbenzyl ammonium chlorideRohm & Haas (3) Hyamine 2389-methyl dodecylbenzyl trimethyl dodecyl xylene bis (trimethyl ammonium chloride) 50% concentrationRohm & Haas (4) Ethoquad 0/25polyoxyethylene oleylmethyl ammonium chloride, 95% concentrationArmour Industrial Chemical Company (B) Pyridinium salts:
(l) Emcol E607N lauroyl colamino formyl methyl (pyridium chloride), 90% concentration- Witco Chemical Company, Inc.
([Il) Anionic:
(A) Alkyl aryl sulfonates:
(l) Suframin 85linear alkyl aryl sodium sulfatc Ultra Division of Watco Chemical Company (2) Stepan DS60desalted sodium dodecyl benzene sulfonateStepan Chemical (3) Stepan AAASammonium salt of dodecyl benzene sulfonateStepan Chemical (B) Alkyl sulfonates:
(1) Petroleum sulfonates (C) Alkyl sulfates:
(l) Stepan0lsodium lauryl sulfate series WA-C,
WA, WAQ
DETAILED DESCRIPTION OF PREFERRED EMBODIMENT The preferred water soluble developer composition of our invention, in its dry form, has the following formula, expressed in percentages by weight:
EXAMPLE Percent Sodium benzoate 55.80 Urea 27.90 EDTA 1.12 Carbowax 4000 13.95 L-77 silicone fluid 0.28 Surfonic LF-l7 0.95
Total 100.00
Carbowax 4000 is a proprietary synthetic, Water-soluble wax having a water solubility of 100 grams per 100 cc.
at 20 C. Other members of the Carbowax series of waxes can be used so long as they are water-soluble, non-volatile and preferably solid at room temperature.
In place of Carbowax 4000 as the film-former, other water-soluble film-formers can be used in the same percentage as that given above and within the ranges given in the broader range formulations, such as: hydroxymethyl cellulose (Methocel H6); sodium earboxymethyl-cellulose (CMC); acacia, or gum arabic; bassorin or tragacanthin (the soluble portion of gum tragacanth); Jagar, a product of Stein-Hall & Co., lnc., said to be a natural vegetable colloid from guar seed; and the like. These film-formers act to produce more uniform small size crystals of the crystalline substance used in the resulting film and to cause such film to adhere well to the test piece surface.
EDTA is the abbreviation for ethylene diamine tetraacetic acid. Other sequestering agents, such as those previously named herein can be employed, especially sodium D-gluconate.
L77 silicone fluid has outstanding wetting and spreading characteristics and can be used by itself at extremely low concentrations (0.05 to 0.10%) by weight of the aqueous solution of the selected crystalline substance or mixture of crystalline substances. Other surfactants, such as those already listed herein, can be used in the same percentage as given in Example 35 or Within the broad range of percentages herein given. Where required in order to prevent embrittlement of the metal of the test piece, the surfactant, as well as the other components of our developer composition, should be substantially or wholly free of sulfur and chlorine.
Algaecides and biocides can be added in low concentrations where desirable or required, for example Hyamin 2389, which is water soluble, non-toxic and functions as a cationic wetting agent. It functions particularly well with L77 silicon fluid. Hyamin 2389 is a mixture of methyl-dodecylbenzyl-trimethyl ammonium chloride, 10% methyldodecylxylene bis-trimethyl ammonium chloride as a aqueous solution, and can be used in concentrations of from 10 to 400 ppm.
The dry composition, e.g. that of Example 35, can be diluted with or dissolved in water to any extent within the broad ranges of percent by weight given in the following example:
The higher the bath concentration, especially of the soluble crystalline substance, the brighter are the fluorescent penetrant indications. A workable concentration of the crystalline substance is obtained by using from A lb. of the dry composition per gallon up to as high as saturation, 3 lbs/gal. of water or even higher. An average solution concentration is 1 lb. of the dry composition per gal. of water.
The water soluble developer of our invention has the following advantages over previously known pigmented developers:
1) It is completely removable by the use of water alone, since the residual developer layer or film after drying is completely soluble in water.
(2) Since there are no particles to keep in suspension, there is no need to agitate the developer bath or container.
(3) There is no problem of geilling or thickening of the developer solution in whatever tank or container it is used in.
(4) Since there are no pigment particles, particle size is not a factor with respect to the sensitivity of the color indication and no masking of indications due to agglomeration of particles.
(5) There are no settling or sludging problems.
It will be understood that modifications and variations may be effected without departing from the scope of the novel concepts of the present invention.
We claim:
1. In a method of detecting surface discontinuities in which a liquid penetrant is applied to the surface of a test piece to become entrapped in any discontinuities therein, the excess of penetrant is removed without removal of penetrant residue entrapped in discontinuities and a developer is thereafter applied to said surface to enhance the visibility of flaw indications including said entrapped penetrant residue, the improvement which comprises:
applying as said developer an aqueous solution consisting essentially of a water-soluble crystalline substance present in an amount of at least 0.5% by weight up to saturation, and
a water dispersible surfactant compatible with said water-soluble crystalline substance and present in an amount from 0.1% to 10% by weight of said solution; said water dispersible surfactant being compatible with said water-soluble crystalline substance upon crystallization of the latter by evaporation of Water from said solution to deposit on said test piece surface a water soluble crystalline film permeable by said penetrant residue to give a flaw indication of enhanced visibility upon inspection thereof.
2. The method as defined by claim 1, in which,
said liquid penetrant is an oil, and
said surfactant is miscible with said oil to effect migration of said penetrant residue into said water soluble film.
3. A method as defined by claim 1, in which said water soluble crystalline substance is an organic compound soluble in water to the extent of 10% by weight of the resulting solution.
4. A method as defined by claim 1, in which said water soluble crystalline substance is an inorganic salt.
5. A method as defined by claim 1, in which said water soluble crystalline substance is a metal salt of an organic acid.
6. A method as defined by claim 1, in which after inspection of said flaw indication said film is removed by water washing to leave a clean surface.
7. A method as defined by claim 1, in which said water soluble crystalline substance is present in an amount of at least 1% by weight, and said surfactant is present in the range of from about 0.1% to 10% by weight of said aqueous solution.
8. A method as defined by claim 1, in which said aqueous solution has a composition within the following proportions by weight of the solution:
water-soluble crystalline substance from 0.5% to saturation.
water-soluble surfactant from 0.1% to 5%, water-soluble film-forming substance from to 10%,
water-soluble sequestering agent from 0 to water-soluble corrosion inhibitor from 0 to 5 and the balance water, said solution upon evaporation leaving a penetrant permeable crystalline film removable by water washing alone.
9. A method as defined by claim 8 wherein,
said water-soluble crystalline substance is sodium benzoate, and
said water-soluble film-forming substance is a normally solid, non-volatile water-soluble wax having a water solubility of 100 grams per 100 cc. at 20 C.
10. An aqueous solution for use as a water-soluble developer in the liquid penetrant method of detecting surface discontinuities in a test piece, consisting essentially of the following:
at least 1% of a mixture of sodium benzoate and urea,
from 0.1% to 5% of a surfactant,
from 0 to 10% of a water-soluble film-former that is non-volatile and solid at room temperature, and the balance water, said solution upon evaporation of the water leaving a water-soluble crystalline film permeable by the liquid penetrant to form a flaw indication of enhanced visibility upon inspection thereof.
11. A water-soluble developer for use in the liquid penetrant method of detecting surface discontinuities in a test piece, comprising an aqueous solution consisting essentially of the following:
from 0.5% to saturation and above of sodium benzoate,
from 0.1% to 10% of a water dispersible surfactant,
a water-soluble film-forming, normally water-soluble wax in an amount up to 10% and sufficient to produce uniformly sized small crystals of said sodium benzoate, from 0 to 5% of a corrosion inhibitor, and the balance being largely water, said solution upon evaporation of the water leaving a water-soluble crystalline film permeable by the liquid penetrant to form a fiaw indication of enhanced visibility upon inspection.
12. An aqueous solution for use as a water-soluble developer in the liquid penetrant method of detecting surface discontinuities in the test piece, consisting essentially 0 of the following:
from 0.5% to saturation of a crystalline water-soluble metal or NH, salt of an organic acid, from 0.1% to 5% of a surfactant, and up to 10% of a water-soluble film-forming, normally solid, non-volatile wax having a water solubility of 100 grams per 100 cc. of water at 20 C. in an amount sufficient to produce uniform small sized crystals of said crystalline salt, the balance being largely water and said solution upon 7 evaporation of said water leaving a water-soluble crystalline film permeable by said liquid penetrant to form a flaw indication of enhanced visibility upon inspection thereof.
(References on following page) References Cited UNITED STATES PATENTS Lemmerman et a1. 252-351 Winning et a1. 252-351 Vitalis 252-3635 Vitalis 252-152 Soule et a1. 252-152 Stephan 252-152 Mains et a1. 252-152 Compton 252-152 Lamberti 252-35] Alburger 250-71 Hirota et a1 73-40 Kakegawa et a1. 252-89 12 FOREIGN PATENTS 7/1949 Canada 254-71 OTHER REFERENCES TOBIAS E. LEVOW, Primary Examiner A. P. DEMERS, Assistant Examiner US. Cl. X.R.
UNI'IEI) S'IA'II'IS PA'IEN'I ()FFNIE CER'IIFICA'IE ()F (IORREC'PION Patent No. 3, 561, 262 Dated February 9 1971 Inventor(s) James S. Borucki 81 Bruce C. Graham It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Col. 2, line 14, cancel "prent" and substitute --present--.
Col. 4, lines 28 81 29, cancel "(to saturation)", and in the column headed by "Percent", after "1" insert --to saturation-.
Col. 4, in Examples 11, 12 and 13, first line under each example, cancel "nitrite" and substitute -nitrate--.
C01. 5, under Example 20, line 49, cancel "(to saturation)" and, same line, after "0.5" add --to saturation--.
C01. 8, line 71, cancel "silicon", and substitute --silicone--.
Col. 9, line 31, correct the spelling of -gel1ing--.
Signed and sealed this 12th day of October 1971.
(SEAL) Attest:
EDWARD M.FLETCHER,JR. ROBERT GOTTSCHALK Attesting Officer Acting Commissioner of Pate
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US67817667A | 1967-10-26 | 1967-10-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3561262A true US3561262A (en) | 1971-02-09 |
Family
ID=24721706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US678176A Expired - Lifetime US3561262A (en) | 1967-10-26 | 1967-10-26 | Water soluble developer |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US3561262A (en) |
| GB (1) | GB1215728A (en) |
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| Publication number | Publication date |
|---|---|
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