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Matched Legal Cases: ['Application No. 60', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14', 'art 14']

Patent US7098463 - Three-dimensional dosimeter for penetrating radiation and method of use - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsThis invention relates to a method of forming a three-dimensional (3D) dosimetric map in a solid translucent or transparent polymer and to an article of manufacture comprising a polymer formulated to capture data imparted by incident penetrating radiation. The present invention provides a method of preparation...http://www.google.com/patents/US7098463?utm_source=gb-gplus-sharePatent US7098463 - Three-dimensional dosimeter for penetrating radiation and method of useAdvanced Patent SearchPublication numberUS7098463 B2Publication typeGrantApplication numberUS 10/790,280Publication dateAug 29, 2006Filing dateMar 1, 2004Priority dateMar 3, 2003Fee statusPaidAlso published asCA2558412A1, EP1599743A2, EP1599743A4, EP2546679A1, US20040211917, WO2004079393A2, WO2004079393A3Publication number10790280, 790280, US 7098463 B2, US 7098463B2, US-B2-7098463, US7098463 B2, US7098463B2InventorsJohn A. AdamovicsOriginal AssigneeHeuris Pharma, LlcExport CitationBiBTeX, EndNote, RefManPatent Citations (38), Non-Patent Citations (36), Referenced by (22), Classifications (8), Legal Events (2) External Links: USPTO, USPTO Assignment, EspacenetThree-dimensional dosimeter for penetrating radiation and method of useUS 7098463 B2Abstract This invention relates to a method of forming a three-dimensional (3D) dosimetric map in a solid translucent or transparent polymer and to an article of manufacture comprising a polymer formulated to capture data imparted by incident penetrating radiation. The present invention provides a method of preparation of a solid translucent or transparent polymer matrix capable of detecting and displaying a dose or doses of penetrating radiation by forming within the polymeric matrix a 3D dosimetric map which is measurable and quantifiable by various known procedures. The dosimetric map is representative of the 3D distribution of the dose or doses of the penetrating radiation to which the polymer had been exposed and can be quantified at high spatial resolution, thereby providing an accurate, stable, storable record in three dimensions of the radiation exposure or dosing event(s).
CROSS-REFERENCED TO RELATED APPLICATION This application claims the benefit of U.S. Provisional Patent Application No. 60/451,826 filed Mar. 3, 2003, the entirety of which is hereby incorporated by reference into this application.
GOVERNMENT INTEREST This invention was made with government support under R43 CA88595-01A2 awarded by the Department of Health and Human Services and the United States Government has certain rights in the invention.
BACKGROUND OF THE INVENTION Dosimeters were developed in order to provide a means of reliably and reproducibly measuring the extent, degree, and distribution of penetration of radiation into media of interest. �Dosimeter� is defined herein as a device designed to undergo changes upon exposure to penetrating radiation, the changes being detectable and quantifiable by the practitioner, and the changes being indicative of the amount and distribution of the incident radiation contained in that exposure. �Penetrating radiation� is defined herein as electromagnetic energy having the form of particles or waves which permeates to some extent a medium of interest in the application. Energy deflected, reflected, or otherwise repelled from the surface of the medium is not penetrating; whereas energy absorbed, transmitted, or in any other sense passing into or through the medium is defined as penetrating. Penetrating radiation may be of natural origin (including, but not limited to sunlight, alpha particles, beta particles, gamma radiation, and other examples of the electromagnetic spectrum) or may be manmade (including, but not limited to neutron radiation, proton radiation, photon radiation, e-beam radiation, high-intensity x-radiation, carbon ion beam radiation, UVA light (400 nm�320 nm), UVB light (320 nm�290 nm), UVC light (290 nm�100 nm), and laser light). It has long been of importance to monitor the extent, degree and distribution of the penetration of this sort of radiation into various media in order to measure and assess the effects of exposure upon materials and humans.
SUMMARY OF THE INVENTION This invention relates to a method of forming a radiation-generated, three-dimensional dosimetric map in a solid translucent or transparent polymer and to an article of manufacture comprising a polymer formulated to capture data imparted by incident penetrating radiation. The present invention provides a method of preparation of a solid translucent or transparent polymer matrix capable of detecting and displaying a penetrating radiation field within the polymeric matrix which is measurable and quantifiable by various known procedures. The 3D dosimetric map thus formed is representative of the 3D energy field to which the plastic had been exposed and can be quantified at high spatial resolution, thereby providing an accurate, stable, storable record in three dimensions of the radiation exposure or dosing event(s).
DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart of a method for fabricating and use of a three-dimensional dosimeter in accordance with the teachings of the present invention.
EXAMPLES Materials used were obtained from the following manufacturers: Crystal Clear 206 Part A, 200 Part B, 220 Part A, 220 Part B from Smooth-On, Inc., Easton, Pa.; carbon tetrachloride, chloroform, bromochloromethane, tribromopropane, dibromohexane, benzoylmethylene blue, benzoyl peroxide, dichloromethane, butyl acetate, 4,4′-methylene bis(cyclohexyl isocyanate) (HMDI), azobis(isobutyrylnitrile), crystal violet lactone, leuco crystal violet, and leucomalachite green from Sigma-Aldrich, St. Louis, Mo.; Poly-Optic 14�70 Part A, Poly-Optic 14�70 Part B, and Optic Part 14X catalyst from PolyTech Development Corp, Easton, Pa.; Andur prepolymers (Andur AL62DP) from Anderson Development Co., Adrian, Mich.; Aliphatic Isocyanate Prepolymer and Z-8002 Polyol from Development Associates, North Kingstown, R.I.; Tolonate XIDT-70B polyisocyanate trimer from Rhodia PPMC; Tone 32B8 Polyol from Dow Chemical Co.; ConOptic 2020 Part A and ConOptic 2020 Part B from Cytec; Hisorb 944 and Hisorb 328 from LG Chem, Ltd.
Example 1 Crystal Clear 206 Part A (250 g), Crystal Clear 206 Part B (200 g), carbon tetrachloride (180 g), Optic Part 14X catalyst (0.6 ml) and leucomalachite green (16 g) were blended thoroughly in a 1000 ml polyethylene beaker until the mixture was homogeneous. The mixture was then immediately poured into molds. The molds were either glass or polyethylene 30 ml vials. The filled molds were then placed under 60 psi pressure and maintained at 25� C. for 18 hours. This was achieved by arranging the molds within a pressure pot of the appropriate size and pressurizing with a compressor pump. At the end of this period, the solid dosimeters formed in polyethylene vials were removed from the molds.
Example 2 In order to assess the dose response of the conversion of the leuco dye of the present invention to the amount of radiation encountered, dosimeters as described in Example 1 were subjected to graded doses of 145 kVp x-rays at three different dose rates, 0.66 Gy/min, 2.17 Gy/min, and 4.4 Gy/min, using Torrex 150D X-ray unit (EG&G, Long Beach, Calif.). The irradiated dosimeters were evaluated using the commercially available OCT-OPUS� CT scanner (MGS Research, Inc., Madison, Conn). In this analysis the conversion of leucomalachite green to the colored species is detected as an increase in optical density at 633 nm, a wavelength at which the leuco dye does not absorb. The transformation of leucomalachite green to its colored form was linear with dose and independent of dose rate.
Example 3 4,4′-methylene bis(cyclohexyl isocyanate) (HMDI) (94 g), carbon tetrachloride (90 g), Crystal Clear 206 Part B (80 g), leucomalachite green (4.0 g) and Optic Part 14� catalyst (1.0 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 4 HMDI (82 g), Andur 62 Polyol (12.8 g) carbon tetrachloride (43 g), a solution of leucomalachite green (1.5 g) in carbon tetrachloride (15 g), Crystal Clear 206 Part B (84 g), and Optic Part 14X catalyst (0.5 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 4 hours. The solid dosimeter was then removed from the mold.
Example 5 HMDI (60 g), Andur 62 Polyol (47.5 g) carbon tetrachloride (35 g), a solution of leucomalachite green (1.5 g) in carbon tetrachloride (15 g), Crystal Clear 206 Part B (82 g), and Optic Part 14X catalyst (0.5 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 4 hours. The solid dosimeter was then removed from the mold.
Example 6 HMDI (406 g), carbon tetrachloride (200 g), leucomalachite green (6.0 g), Crystal Clear 206 Part B (350 g), and Optic Part 14X catalyst (1.0 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 1000 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 7 Anderson Development Inc. Andur AL62DP aliphatic Isocyanate Prepolymer (380 g), carbon tetrachloride (200 g), Z-8002 Part A Polyol (380 g), and leucomalachite green (6.0 g) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 1000 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 8 Tolonate XIDT-70B (70% solution in butyl acetate, 248.5 g), Crystal Clear 206 Part B (97 g), carbon tetrachloride (93 g), leucomalachite green (13 g) and Optic Part 14X catalyst (0.4 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 1000 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 9 Crystal Clear 206 Part A (135 g), Crystal Clear 206 Part B (112 g), chloroform (80 g), leucomalachite green (10 g), and Optic Part 14X catalyst (0.5 ml) were blended thoroughly in a 500 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 10 Crystal Clear 206 Part A (135 g), Crystal Clear 206 Part B (112 g), chloroform (80 g), crystal violet lactone (10 g), and Optic Part 14X catalyst (0.5 ml) were blended thoroughly in a 500 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 11 Tinuvin (2.8 g) was dissolved in carbon tetrachloride (340.9 g) and HMDI (500.0 g) was added. This solution was blended thoroughly with Tone 32B8 (1624.1 g), leucomalachite green (32.4 g) and Optic Part 14X catalyst (1.0 ml). The mixture was then immediately poured into mold fabricated from an 800 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 4 hours. The solid dosimeter was then removed from the mold.
Example 12 Z-8002 Part B Isocyanate (200 g), Cytec Polyol (200 g), carbon tetrachloride (90 g), and leucomalachite green (9 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from an 800 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 4 hours. The solid dosimeter was then removed from the mold.
Example 13 Tolonate XIDT-70B (70% solution in butyl acetate, 250 g), Crystal Clear 206 Part B (100 g), carbon tetrachloride (94 g), leucomalachite green (9.4 g) and Optic Part 14X catalyst (0.4 ml) were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 1000 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 1.5 hours. The molded dosimeter was then warmed at 50� C. for 18 hours. The solid dosimeter was then removed from the mold.
Example 14 Poly-Optic 14�70 Part A (100 g), Poly-Optic 14�70 Part B (125 g), carbon tetrachloride (39.8 g), and leucomalachite green (10.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 15 Poly-Optic 14�70 Part A (102.7 g), Poly-Optic 14�70 Part B (123.2 g), bromochloromethane (19.3 g), and leucomalachite green (10.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 16 Poly-Optic 14�70 Part A (103.4 g), Poly-Optic 14�70 Part B (126.6 g), tribromopropane (55.2 g), and leucomalachite green (10.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 17 Poly-Optic 14�70 Part A (104.8 g), Poly-Optic 14�70 Part B (126.0 g), 1,6-dibromohexane (47.6 g), and leucomalachite green (10.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 18 Poly-Optic 14�70 Part A (107.5 g), Poly-Optic 14�70 Part B (129.6 g), bromochloromethane (77.2 g), carbon tetrachloride (3.2 g) and benzoylmethylene blue (5.03 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 19 Poly-Optic 14�70 Part A (45 g), Poly-Optic 14�70 Part B (45 g), tetrahydrofuran (5.0 ml), benzoyl peroxide (1.0 ml), and leucomalachite green (4.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 20 Poly-Optic 14�70 Part A (80 g), Poly-Optic 14�70 Part B (100 g), tetrahydrofuran (7.0 ml), a solution of azobis(isobutyrylnitrile) (0.29 g) in tetrahydrofuran (0.2 ml), and leucomalachite green (4.0 g) were blended thoroughly. The mixture was then immediately poured into mold fabricated from a 400 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 24 hours. The solid dosimeter was then removed from the mold.
Example 21 Crystal Clear 206 Part A (100 g), Crystal Clear 206 Part B (100 g), tetrachloroethane (47.9 g), Pergascript Blue I-2R (3 g), were blended thoroughly in a 500 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 72 hours. The solid dosimeter was then removed from the mold.
Example 22 Crystal Clear 206 Part A (150 g), Crystal Clear 206 Part B (150 g), tetrachloroethane (112 g), Pergascript Blue SRB-P (10 g), were blended thoroughly in a 500 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 500 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 72 hours. The molded dosimeters were then warmed at 50� C. for 6 hours. The solid dosimeter was then removed from the mold.
Example 23 ConOptic 2020 Part A (100 g), ConOptic 2020 Part B (100 g), tetrachloroethane (45 g), and leucomalachite green (3.9 g) were blended thoroughly in a 500 ml polyethylene beaker. The mixture was then immediately poured into 30 ml glass vials. The filled molds were pressurized as in Example 1 and incubated at 25� C. for 72 hours. The dosimeters were irradiated as in Example 2 at 4.4 Gy/min, resulting in the development of a clearly visible dosimetric map. The dosimeters were then warmed in an oven at 50� C. for 20 minutes. During this time the exposed areas of the dosimeters were completely bleached and the dosimetric data was erased. The irradiation-bleaching process was repeated twice more on the same set of dosimeters. Each time the irradiation resulted in a clearly visible dosimetric map, and the bleaching completely erased the data.
Example 24 Crystal Clear 206 Part A (260 g), Crystal Clear 206 Part B (200 g), tetrachloroethane (104 g), leucomalachite green (10 g), Optic Part 14X catalyst (0.2 ml), and Hisorb 944 were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was then immediately poured into mold fabricated from a 1000 ml cylindrical polyethylene beaker. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 20 hours. The solid dosimeter was then removed from the mold.
Example 25 Crystal Clear 206 Part A (1048 g), Crystal Clear 206 Part B (800 g), tetrachloroethane (480 g), leucomalachite green (40 g), Optic Part 14X catalyst (1.0 ml), and Hisorb 328 (2 g) were blended thoroughly in a 2000 ml polyethylene beaker. The mixture was then immediately poured into a polyethylene mold having the size and shape of the average human brain. The filled mold was pressurized as in Example 1 and incubated at 25� C. for 36 hours. The molded dosimeter was warmed to 40� C. for 48 hours. The solid dosimeter was then removed from the mold.
Example 26 HMDI (280 g), Crystal Clear 206 Part B (242 g), methylene chloride (162 g), Pergascript Blue SRB-P (16 g), Optic Part 14X catalyst (0.5 ml), were blended thoroughly in a 1000 ml polyethylene beaker. The mixture was filtered through a 10 μm filter and pressurized as in Example 1 and incubated at 25� C. for 20 hours.
Example 27 HMDI (66 g), Crystal Clear 206 Part B (58 g), chloroform (10 g), carbon tetrachloride (27 g), leuco crystal violet (3.8 g), Optic Part 14X catalyst (0.2 ml), were blended thoroughly in a 100 ml polyethylene beaker. The mixture was filtered through a 10 μm filter and pressurized as in Example 1 and incubated at 25� C. for 20 hours.
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