US3684018A - Foam-forming flame-extinguishing compositions containing alkylpolyalkoxysulfates, polyoxyethylene resin and symmetrical dibromotetrafluoroethane - Google Patents
Foam-forming flame-extinguishing compositions containing alkylpolyalkoxysulfates, polyoxyethylene resin and symmetrical dibromotetrafluoroethane Download PDFInfo
- Publication number
- US3684018A US3684018A US109620A US3684018DA US3684018A US 3684018 A US3684018 A US 3684018A US 109620 A US109620 A US 109620A US 3684018D A US3684018D A US 3684018DA US 3684018 A US3684018 A US 3684018A
- Authority
- US
- United States
- Prior art keywords
- foam
- percent
- dibromotetrafluoroethane
- weight
- extinguishing
- 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
- 239000000203 mixture Substances 0.000 title claims abstract description 45
- 239000011347 resin Substances 0.000 title claims abstract description 23
- 229920005989 resin Polymers 0.000 title claims abstract description 23
- -1 polyoxyethylene Polymers 0.000 title claims abstract description 22
- 229920003171 Poly (ethylene oxide) Polymers 0.000 title claims abstract description 21
- JLGADZLAECENGR-UHFFFAOYSA-N 1,1-dibromo-1,2,2,2-tetrafluoroethane Chemical compound FC(F)(F)C(F)(Br)Br JLGADZLAECENGR-UHFFFAOYSA-N 0.000 title 1
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- KVBKAPANDHPRDG-UHFFFAOYSA-N dibromotetrafluoroethane Chemical compound FC(F)(Br)C(F)(F)Br KVBKAPANDHPRDG-UHFFFAOYSA-N 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 3
- 239000006260 foam Substances 0.000 description 11
- 239000004088 foaming agent Substances 0.000 description 8
- 239000003380 propellant Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 150000003863 ammonium salts Chemical class 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 238000009434 installation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000004604 Blowing Agent Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 125000006353 oxyethylene group Chemical group 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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
- 241001349296 Tragia volubilis Species 0.000 description 1
- BIDRONFUNLAMOH-UHFFFAOYSA-N [BrH]1[BrH]CC=C1 Chemical compound [BrH]1[BrH]CC=C1 BIDRONFUNLAMOH-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- DIORMHZUUKOISG-UHFFFAOYSA-N sulfoformic acid Chemical class OC(=O)S(O)(=O)=O DIORMHZUUKOISG-UHFFFAOYSA-N 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0071—Foams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
Definitions
- ABSTRACT A foam-forming flame-extinguishing composition containing an aqueous solution of a water soluble alkylpolyalkoxy-sulfates, preferably in combination with a polyoxyethylene resin and advantageously, with symmetrical-d1bromotetrafluoroethane.
- Our present invention relates to foam-forming flameextinguishing compositions and, more particularly, to flame-extinguishing compositions particularly adapted to quench, extinguish or confine fires fueled by hydrocarbons.
- foam-forming flame-extinguishing compositions have been inadequate for extinguishing fires fueled by hydrocarbons as may develop at industrial installations, refineries, tank farms and with the like, and burning hydrocarbons on water.
- a flame-extinguishing foam-forming liquid composition which contains one or more fluorobromoalkanes in addition to the substances commonly provided in flame-extinguishing foams.
- fluorobromoalkanes included water, emulsifying and foam-stabilizing surface active agents, propellants and foaming agents, antifreezing agents capable of lowering the freezing point of the composition, buffering agents, corrosion inhibitors and thickening and carrying agents.
- the surface-active agents have been found to be most suitable as the organic sulfonates and sulfates, alkylarylpolyethyleneglycol ethers, esters of alcohol such as sorbitol with higher fatty acids such as lauric, stearic, palrnitic acids, sodium or ammonium salts or sulfocarboxylic acids such as dialkylsulfosuccinic acid with up to eight carbon atoms in each alkyl group.
- composition can be improved by associating with the bromofluoroalkane a foaming agent of the ammonium alkylpolyalkoxysulfate type to produce a binary combination with the bromofluoroalkane.
- the binary combination used as an aqueous solution or dispersion, provided markedly improved results.
- alkylpolyalkoxysulfate in the form of water-soluble salts constitute excellent flame-extinguishing substances in their own right, especially when dispersed as a foam upon a hydrocarbon fire.
- the alkylpolyalkoxysulfate is used as an ammonium salt, possesses ethoxy groups in a chain of two to 30 ethoxy groups and has an alkyl group with eight to 22 carbon atoms, preferably 12-14. Best results are obtained with ammonium]aurylpolyethoxysulfate.
- ammoniumlaurylpolyethoxysulfate acts synergistically or symbiotically with water-soluble high molecular weight polyoxyethlene resins in creating flame-extinguishing foams under the action of a blowing agent or propellant.
- the fire-fighting properties of a water-soluble surface active substance capable of generating foam under the action of a blowing agent, especially the ammoniumalkylpolyalkoxysulfate are greatly improved by the addition to the solution of the water-soluble high-molecular weight polyoxyethylene resin.
- compositions of the present invention may also contain propellants, dispersing agents and other conventional adjuvants, such as corrosion inhibitors and anti-freezing agents, in the amounts and of the type described in the aforementioned copending application.
- a preferred subgroup of water-soluble alkylpolyalkoxysulfate is the ammonium salts of alxylpolyethoxy sulfuric acids in which the alkyl radical contains 12 to 14 atoms in the main chain and the number of ethoxy groups is two to 30 as noted earlier. Because the ammoniumalkylpolyalkoxysulfates generally have peculiar foaming characteristics, it has been found to be advantageous to use the ammonium salt of lauryltriethoxysulfate, commonly in the form of a water solution containing 10 percent by weight of the active substance.
- the polyoxyethylene resin is a polymer having 7,000 to 200,000 oxyethylene units per molecule, an average molecular weight of 250,000 to 8,000,000, and a viscosity of 5,000 to 8,000 cps in an 0.5 to 5 percent aqueous solution.
- the liquid composition of the present invention may comprise the three active components individually or in combination, together making up 2 to 70 percent by weight of the composition, the balance being water and adjuvants as noted earlier.
- ammoniumlauryltriethoxysulfate and the polyoxyethylene are used together, they are present in a ratio by weight of 2 to 0.5 while dibromotetrafluoroethane may be employed in an amount of 3.5 to 35 times the total weight of the ammonium salt and the polyoxyethylene resin.
- the flame-extinguishing material has the following composition:
- composition of the present invention may be projected onto the fire site with conventional foam-throwing apparatus to which the components of the composition are fed separately and are combined at the nozzle under the action of the propellant or blowing agent. It has been found that, for practical use in mobile fire-extinguishing installations,
- a mixture containing an aqueous solution of ammoniurnlaurylpolyethyoxysulfate and the polyoxyethylene resin should be provided in one tank while the dibrotetrafluoroethane is supplied in another tank, the contents of the tanks being fed to the foam-projecting nozzle together with a blowing agent such as carbon dioxide or one of the other propellants set forth in the above-identified co-pending application.
- a blowing agent such as carbon dioxide or one of the other propellants set forth in the above-identified co-pending application.
- the fuel was ignited and pennitted to burn; after 60 seconds of precombustion, a single operator began to extinguish the fire with an aqueous foam-forming composition. The fire was completely extinguished within 60 seconds.
- Example II was repeated, but with a mixture of 400 liters of gasoline and liters of kerosene as the fuel. The fuel was ignited and let burn for 60 seconds; after this precombustion period, the fire was put out within 23 seconds, using the following liquid composition:
- EXAMPLE lV a) l ,Z-dibromo- 1 l ,2,2-tetrailuoroethane kg8 b) aqueous solution of the two components cited in Example 111, 1:1 by volume kg2.2 c) water kg22 extinguished the tire within 22 seconds (expansion ratio, as previously defined, 1:10).
- a flame-extinguishing foam-forming composition comprising as active fire-extinguishing components, 1 ,2-dibromotetrafluoroethane, ammoniumlauryltriethoxysulfate and a polyoxyethylene resin, in aqueous solution, of an average molecular weight of 250,000 to 8,000,000.
- composition defined in claim 2 wherein said polyoxyethylene resin has a viscosity in 0.5 to 5 percent aqueous solution of 5,000 to 8,000 cPs.
- composition defined in claim 4 consisting essentially of l to 10 percent by weight of a 10 percent aqueous solution of arnmoniumlauryltriethoxysulfate, 1 to 10 percent by weight of a 0.5 to 5 percent aqueous solution of said polyoxyethlene resin, 2 to 70 percent by weight 1,2-dibromotetrafluoroethane, and 10 to 98 percent by weight water.
- a method of extinguishing a hydrocarbon fire comprising the step of projecting the foaming composition defined in claim 5 thereupon.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Fire-Extinguishing Compositions (AREA)
- Liquid Carbonaceous Fuels (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT1982770 | 1970-01-27 | ||
| IT1992170 | 1970-01-29 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3684018A true US3684018A (en) | 1972-08-15 |
Family
ID=26327322
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US109620A Expired - Lifetime US3684018A (en) | 1970-01-27 | 1971-01-25 | Foam-forming flame-extinguishing compositions containing alkylpolyalkoxysulfates, polyoxyethylene resin and symmetrical dibromotetrafluoroethane |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US3684018A (enrdf_load_html_response) |
| BE (1) | BE762012A (enrdf_load_html_response) |
| DE (1) | DE2103385A1 (enrdf_load_html_response) |
| FR (1) | FR2077046A5 (enrdf_load_html_response) |
| GB (1) | GB1311602A (enrdf_load_html_response) |
| NL (1) | NL7100798A (enrdf_load_html_response) |
| NO (1) | NO130299B (enrdf_load_html_response) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3888641A (en) * | 1972-07-24 | 1975-06-10 | Nittan Co Ltd | Method of erasing smoke |
| US4402364A (en) * | 1981-12-17 | 1983-09-06 | Max Klein | Fire extinguishing method |
| US4446923A (en) * | 1979-04-30 | 1984-05-08 | Walter Kidde & Co., Inc. | Removal of explosive or combustible gas or vapors from tanks and other enclosed spaces |
| US5080177A (en) * | 1990-07-26 | 1992-01-14 | Great Lakes Chemical Corporation | Fire extinguishing methods utilizing 1-bromo-1,1,2,2-tetra-fluoroethane |
| US5258137A (en) * | 1984-12-24 | 1993-11-02 | The Dow Chemical Company | Viscoelastic surfactant based foam fluids |
| WO1994009852A1 (en) * | 1992-03-09 | 1994-05-11 | The Dow Chemical Company | Viscoelastic surfactant based foam fluids |
| US5945025A (en) * | 1997-12-08 | 1999-08-31 | Cunningham; James A. | Fire extinguishing composition and method for fire extinguishing |
| US20070085060A1 (en) * | 2005-10-18 | 2007-04-19 | Dario Santoro | Method of making a fire extinguishing chemical |
| US20100330290A1 (en) * | 2006-12-19 | 2010-12-30 | Francis Dobler | Curtain coating method using edge guide fluid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2653130A (en) * | 1951-05-17 | 1953-09-22 | Du Pont | Fire extinguishing composition of cbrf or cfbrcfbr containing cf as a propellant |
| US3186943A (en) * | 1961-12-11 | 1965-06-01 | Safety Dev Corp | Foam method for atmosphere control |
| US3258423A (en) * | 1963-09-04 | 1966-06-28 | Richard L Tuve | Method of extinguishing liquid hydrocarbon fires |
| US3422011A (en) * | 1966-05-03 | 1969-01-14 | Kidde & Co Walter | Foam producing material |
| US3479286A (en) * | 1965-09-22 | 1969-11-18 | Montedison Spa | Flame-extinguishing compositions |
| US3562156A (en) * | 1969-06-12 | 1971-02-09 | Minnesota Mining & Mfg | Fire extinguishing composition comprising a fluoroaliphatic surfactant and a fluorine-free surfactant |
| US3579446A (en) * | 1968-04-29 | 1971-05-18 | Minimax Ag | Fire-extinguishing foam composition including a basic,nitrogenous compound |
-
1971
- 1971-01-21 NO NO00217/71A patent/NO130299B/no unknown
- 1971-01-21 NL NL7100798A patent/NL7100798A/xx unknown
- 1971-01-25 US US109620A patent/US3684018A/en not_active Expired - Lifetime
- 1971-01-25 BE BE762012A patent/BE762012A/xx unknown
- 1971-01-26 DE DE19712103385 patent/DE2103385A1/de active Pending
- 1971-01-27 FR FR7102693A patent/FR2077046A5/fr not_active Expired
- 1971-04-19 GB GB2029471A patent/GB1311602A/en not_active Expired
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2653130A (en) * | 1951-05-17 | 1953-09-22 | Du Pont | Fire extinguishing composition of cbrf or cfbrcfbr containing cf as a propellant |
| US3186943A (en) * | 1961-12-11 | 1965-06-01 | Safety Dev Corp | Foam method for atmosphere control |
| US3258423A (en) * | 1963-09-04 | 1966-06-28 | Richard L Tuve | Method of extinguishing liquid hydrocarbon fires |
| US3479286A (en) * | 1965-09-22 | 1969-11-18 | Montedison Spa | Flame-extinguishing compositions |
| US3422011A (en) * | 1966-05-03 | 1969-01-14 | Kidde & Co Walter | Foam producing material |
| US3579446A (en) * | 1968-04-29 | 1971-05-18 | Minimax Ag | Fire-extinguishing foam composition including a basic,nitrogenous compound |
| US3562156A (en) * | 1969-06-12 | 1971-02-09 | Minnesota Mining & Mfg | Fire extinguishing composition comprising a fluoroaliphatic surfactant and a fluorine-free surfactant |
Non-Patent Citations (1)
| Title |
|---|
| Polyox Water Soluble Resins, Union Carbide Company, New York, 1968 P. 1 4. * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3888641A (en) * | 1972-07-24 | 1975-06-10 | Nittan Co Ltd | Method of erasing smoke |
| US4446923A (en) * | 1979-04-30 | 1984-05-08 | Walter Kidde & Co., Inc. | Removal of explosive or combustible gas or vapors from tanks and other enclosed spaces |
| US4402364A (en) * | 1981-12-17 | 1983-09-06 | Max Klein | Fire extinguishing method |
| US5258137A (en) * | 1984-12-24 | 1993-11-02 | The Dow Chemical Company | Viscoelastic surfactant based foam fluids |
| US5080177A (en) * | 1990-07-26 | 1992-01-14 | Great Lakes Chemical Corporation | Fire extinguishing methods utilizing 1-bromo-1,1,2,2-tetra-fluoroethane |
| WO1994009852A1 (en) * | 1992-03-09 | 1994-05-11 | The Dow Chemical Company | Viscoelastic surfactant based foam fluids |
| US5945025A (en) * | 1997-12-08 | 1999-08-31 | Cunningham; James A. | Fire extinguishing composition and method for fire extinguishing |
| US20070085060A1 (en) * | 2005-10-18 | 2007-04-19 | Dario Santoro | Method of making a fire extinguishing chemical |
| US20100330290A1 (en) * | 2006-12-19 | 2010-12-30 | Francis Dobler | Curtain coating method using edge guide fluid |
Also Published As
| Publication number | Publication date |
|---|---|
| BE762012A (fr) | 1971-07-26 |
| DE2103385A1 (de) | 1971-07-29 |
| NO130299B (enrdf_load_html_response) | 1974-08-12 |
| NL7100798A (enrdf_load_html_response) | 1971-07-29 |
| FR2077046A5 (enrdf_load_html_response) | 1971-10-15 |
| GB1311602A (en) | 1973-03-28 |
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