US5326585A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method and compositions for manufacture of chemical sensors
Assignee: Puritan Bennett Corp
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Filing: 1993-08-17
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Granted: 1994-07-05
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Expires: 2013-08-17
Abstract
Abstract The method for making an optical fiber microsensor involves applying an uncured analyte sensing matrix to an optical fiber and crosslinking the sensing matrix in situ on the optical fiber to yield an ion permeable microsensor which can be used intravascularly to monitor pH, or partial pressures of oxygen or carbon dioxide in blood. The liquid form of the sensing matrix contains a crosslinking agent and a crosslinking inhibitor which can be removed by exposure to elevated temperatures to allow the sensing matrix to crosslink and cure as desired, in situ, on the surface of the optical fiber. A liquid crosslinking overcoat layer containing a crosslinking agent and a crosslinking inhibitor which can be removed by exposure to heat can also be applied over the cured sensing matrix.
Inventors
- 👤 Alan M. Nelson
- 👤 Carmen L. Soikowski
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 10:25
CPC Classifications
G; G01; G01N; G01N21/00; G01N21/75; G01N21/77; G01N21/7703; G01N2021/7706; G01N2021/773; G01N2021/7769; G01N2021/7786
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
145 words
A method of making an analyte sensor including an optical fiber having a surface portion covered with a polymeric analyte sensing matrix including a dye indicator material, comprising the steps of: preparing an analyte permeable polymer with an analyte sensitive indicator dye covalently bonded to the analyte permeable polymer to form a liquid polymeric analyte sensing matrix; forming a liquid mixture of said liquid polymeric analyte sensing matrix with a crosslinking agent and a crosslinking inhibitor which can be removed by exposure to heat; coating said optical fiber surface portion with said liquid mixture; and heating said liquid mixture on said optical fiber surface portion for a sufficient period of time to remove said crosslinking inhibitor from said liquid mixture, whereby said crosslinking agent crosslinks said liquid polymeric analyte sensing matrix in situ on said optical fiber surface portion thereby producing a cured sensing matrix.
Claim 2
Independent Claim
145 words
A method of making an analyte sensor including an optical fiber having a surface portion covered with a polymeric analyte sensing matrix including a dye indicator material, comprising the steps of: preparing an analyte permeable polymer with an analyte sensitive indicator dye covalently bonded to the analyte permeable polymer to form a liquid polymeric analyte sensing matrix; forming a liquid mixture of said liquid polymeric analyte sensing matrix with a crosslinking agent and a crosslinking inhibitor which can be removed by exposure to heat; coating said optical fiber surface portion with said liquid mixture; and heating said liquid mixture on said optical fiber surface portion for a sufficient period of time to remove said crosslinking inhibitor from said liquid mixture, whereby said crosslinking agent crosslinks said liquid polymeric analyte sensing matrix in situ on said optical fiber surface portion thereby producing a cured sensing matrix.
Claim 3
Dependent Claim
55 words
The method of claim 1, wherein said crosslinking agent comprises a blocked polyether isocyanate incorporating said crosslinking inhibitor selected from the group consisting of ethanol, o-nitrophenol, resorcinol, benzenethiol, acetyl acetone, 2-methyl-2-propanol, p-chlorophenol, phloroglucinol, ethyl acetoacetate, acetone oxime, methyl ethyl ketone oxime, m-cresol, guaiacol, 1-dodecanthiol, diethyl malonate, diphenyl amine, phenol caprolactam, 2, 4-diisobutylphenol, monomethylaniline, and isoocytylphenol.
Claim 4
Dependent Claim
12 words
The method of claim 2, wherein said crosslinking inhibitor is acetone oxime.
Claim 5
Dependent Claim
22 words
The method of claim 2, wherein said liquid polymeric analyte sensing matrix comprises a copolymer of hydroxyethyl methacrylate and N-(3-aminopropyl) methacrylate hydrochloride.
Claim 6
Dependent Claim
16 words
The method of claim 4, wherein said dye indicator material comprises 8-hydroxy-1, 3, 6 pyrenetrisulfonic acid.
Claim 7
Dependent Claim
33 words
The method of claim 1, wherein said liquid polymeric analyte sensing matrix comprises a crosslinkable vinyl terminated organosiloxane, said crosslinking agent comprises a catalyst and said crosslinking inhibitor comprises a vinyl terminated dimethylsiloxane.
Claim 8
Dependent Claim
14 words
The method of claim 6, wherein said crosslinking inhibitor has the chemical structure ##STR4##
Claim 9
Dependent Claim
12 words
The method of claim 6, wherein said crosslinking inhibitor is divinyl tetramethyldisiloxane.
Claim 10
Dependent Claim
24 words
The method of claim 6, wherein said dye indicator material is selected from the group consisting of fluorescein and 8-hydroxy-1, 3, 6 pyrenetrisulfonic acid.
Claim 11
Dependent Claim
35 words
The method of claim 9, wherein said dye indicator material is covalently bonded with a copolymer selected from the group consisting of acrylamide, hydroxyethyl methacrylate, and a copolymer of hydroxyethyl methacrylate and N-(3-aminopropyl) methacrylate hydrochloride.
Claim 12
Dependent Claim
24 words
The method of claim 6, wherein said dye indicator material is selected from the group consisting of coronene and decacyclene, and a combination thereof.
Claim 13
Dependent Claim
15 words
The method of claim 9, wherein said liquid polymeric analyte sensing matrix comprises methylhydrodimethylsiloxane copolymer.
Claim 14
Dependent Claim
21 words
The method of claim 6, wherein said dye indicator material comprises a polynuclear aromatic dye covalently linked to the organosiloxane copolymer.
Claim 15
Dependent Claim
32 words
The method of claim 1, wherein said liquid mixture on said optical fiber surface portion is heated to a temperature exceeding the boiling point or temperature of decomposition of said crosslinking inhibitor.
Claim 16
Dependent Claim
32 words
The method of claim 1, wherein said liquid mixture on said optical fiber surface portion is exposed to a temperature of from about 140° to about 240° C. for approximately 10-60 seconds.
Claim 17
Dependent Claim
28 words
The method of claim 1, wherein said liquid mixture on said optical fiber surface portion is exposed to a temperature of about 220° C. for approximately 15 seconds.
Claim 18
Dependent Claim
27 words
The method of claim 1, wherein said liquid mixture on said optical fiber surface portion is exposed to a temperature of about 175° for approximately 20 seconds.
Claim 19
Dependent Claim
97 words
The method of claim 1, further including the step of applying a layer of an uncured overcoat mixture comprising a second crosslinking agent and a second crosslinking inhibitor which can be removed by exposure to elevated temperature over said liquid polymeric analyte sensing matrix following said step of heating said liquid mixture; and heating said uncured overcoat mixture on said optical fiber surface portion for a sufficient period of time to remove said second crosslinking inhibitor from said uncured overcoat mixture, whereby said second crosslinking agent crosslinks said overcoat mixture in situ over said cured sensing matrix.
Claim 20
Dependent Claim
12 words
The method of claim 18, wherein said overcoat mixture includes titanium dioxide.
Claim 21
Dependent Claim
62 words
The method of claim 18, wherein said overcoat second crosslinking agent comprises a blocked form of a polyether isocyanate incorporating said second crosslinking inhibitor, and said second crosslinking inhibitor is selected from the group consisting of ethanol, o-nitrophenol, resorcinol, benzenethiol, acetyl acetone, 2-methyl-2-propanol, p-chlorophenol, phloroglucinol, ethyl acetoacetate, acetone oxime, m-cresol, guaiacol, 1-dodecanthiol, diethyl malonate, diphenyl amine, phenol caprolactam, 2,4-diisobutylphenol, monomethylaniline, and isooctylphenol.
Claim 22
Dependent Claim
14 words
The method of claim 18, wherein said overcoat second crosslinking inhibitor comprises acetone oxime.
Claim 23
Dependent Claim
30 words
The method of claim 18, wherein said overcoat second crosslinking agent comprises a crosslinkable vinyl terminated organosiloxane and a catalyst, and said second crosslinking inhibitor comprises a vinyl terminated dimethylsiloxane.
Claim 24
Dependent Claim
15 words
The method of claim 22, wherein said second crosslinking inhibitor has the chemical structure ##STR5##
Claim 25
Dependent Claim
13 words
The method of claim 22, wherein said second crosslinking inhibitor is divinyl tetramethyldisiloxane.
Claim 26
Dependent Claim
12 words
The method of claim 22, wherein said overcoat mixture comprises methylhydrodimethylsiloxane copolymer.
Claim 27
Dependent Claim
33 words
The method of claim 18, wherein said uncured overcoat mixture on said cured sensing matrix is heated to a temperature exceeding the boiling point or temperature of decomposition of said second crosslinking inhibitor.
Claim 28
Dependent Claim
28 words
The method of claim 18, wherein said uncured overcoat mixture on said cured sensing matrix is exposed to a temperature of from about 140° to about 220° C.
Claim 29
Dependent Claim
34 words
The method of claim 18, wherein said uncured overcoat mixture on said cured sensing matrix is exposed to a temperature of from about 140° to about 220° C. for approximately 10 to 60 seconds.
Claim 30
Dependent Claim
27 words
The method of claim 18, wherein said uncured overcoat mixture on said cured sensing matrix is exposed to a temperature of about 175° for approximately 30 seconds.
Claim 31
Dependent Claim
51 words
The method of claim 1, further including the step of priming said optical fiber surface portion by applying a silanizing agent selected from the group consisting of isocyanatopropyltriethoxysilane and vinyltriethoxysilane to said optical fiber surface portion prior to said step of coating said optical fiber surface portion with said liquid mixture.
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