US5262192A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method and compositions for manufacture of chemical sensors
Assignee: Puritan Bennett Corp
•
Filing: 1992-04-27
•
Granted: 1993-11-16
•
Expires: 2012-04-27
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
2026-11-06 04:34
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: 22
Claim 1
Independent Claim
142 words
A method of making an analyte sensor including an optical fiber having a surface portion covered with a polymer analyte sensing matrix including a dye indicator material, comprising the steps of: preparing a copolymer of hydroxyethyl methacrylate and N-(3-aminopropyl) methacrylate and covalently bonding said dye indicator material to said copolymer to form a liquid polymer 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 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
142 words
A method of making an analyte sensor including an optical fiber having a surface portion covered with a polymer analyte sensing matrix including a dye indicator material, comprising the steps of: preparing a copolymer of hydroxyethyl methacrylate and N-(3-aminopropyl) methacrylate and covalently bonding said dye indicator material to said copolymer to form a liquid polymer 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 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
54 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 isooctylphenol.
Claim 4
Dependent Claim
12 words
The method of claim 2, wherein said crosslinking inhibitor is acetone oxime.
Claim 5
Dependent Claim
16 words
The method of claim 1, wherein said dye indicator material comprises 8-hydroxy-1, 3, 6 pyrenetrisulfonic acid.
Claim 6
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 7
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 8
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 9
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 10
Dependent Claim
89 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 heat over said analyte cured sensing matrix mixture; and then 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 11
Dependent Claim
12 words
The method of claim 9, wherein said overcoat mixture includes titanium dioxide.
Claim 12
Dependent Claim
56 words
The method of claim 9, wherein said second crosslinking agent comprises a blocked polyether isocyanate incorporating said second 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 isooctylphenol.
Claim 13
Dependent Claim
13 words
The method of claim 9, wherein said second crosslinking inhibitor comprises acetone oxime.
Claim 14
Dependent Claim
29 words
The method of claim 9, wherein said second crosslinking agent comprises a crosslinkable vinyl terminated organosiloxane and a catalyst, and said second crosslinking inhibitor comprises a vinyl terminated dimethylsiloxane.
Claim 15
Dependent Claim
15 words
The method of claim 13, wherein said second crosslinking inhibitor has the chemical structure ##STR3##
Claim 16
Dependent Claim
13 words
The method of claim 13, wherein said second crosslinking inhibitor is divinyl tetramethyldisiloxane.
Claim 17
Dependent Claim
13 words
The method of claim 13, wherein said overcoat mixture further comprises methylhydrodimethylsiloxane copolymer.
Claim 18
Dependent Claim
32 words
The method of claim 9, 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 crosslinking inhibitor.
Claim 19
Dependent Claim
28 words
The method of claim 9, wherein said uncured overcoat mixture on said cured sensing matrix is exposed to a temperature of from about 140° to about 220° C.
Claim 20
Dependent Claim
34 words
The method of claim 9, 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 21
Dependent Claim
27 words
The method of claim 9, wherein said uncured overcoat mixture on said cured sensing matrix is exposed to a temperature of about 175° for approximately 30 seconds.
Claim 22
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.
References Cited (Backward Citations)
US4446293A
Cited
US4557900A
Cited
US4671937A
Cited
US4752115A
Cited
US4861727A
Cited
US4824789A
Cited
US4798738A
Cited
US4824789B1
Cited
US4867919A
Cited
US4886338A
Cited
US4714770A
Cited
US4712865A
Cited
WO1988005533A1
Cited
US4746751A
Cited
US4842783A
Cited
US4925268A
Cited
EP0363993A2
Cited
US5056520A
Cited
US5132057A
Cited
US5152287A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1996-11-15 | 1997-05-17 | 1997-11-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-11-15 | 2001-05-17 | 2001-11-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-11-15 | 2005-05-17 | 2005-11-16 | $7700.00 | Window Closed / Lapsed |