US3589172A
Expired / Lapsed
US
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Method and apparatus for characterizing materials
Assignee: New Jersey Zinc Co
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Filing: 1967-01-12
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Granted: 1971-06-29
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Expires: 1987-01-12
Abstract
Abstract A novel process for characterizing compositions of matter is described in which a sample of the unknown material is heated and the rate of gas evolution from the sample is measured. Comparison of the temperature-gas evolution rates or profiles of the unknown material with the rates or profiles obtained from known materials provides identification of the unknown. Apparatus for carrying out the process is also described.
Inventors
- 👤 Robert S Bowman
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 02:20
CPC Classifications
G; G01; G01N; G01N7/00; G01N7/14
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
23 words
A method according to claim 1, wherein the sample is heated at a rate between about 1* and about 50* C. per minute.
Claim 2
Dependent Claim
22 words
A method according to claim 1, wherein the sample is heated at a rate between about 5* and 10* C. per minute.
Claim 3
Dependent Claim
35 words
A method according to claim 1, wherein said sample is evacuated in step (a) prior to heating in step (b) to a vacuum between about 10 2 mm. to 10 4 mm. of mercury absolute.
Claim 4
Dependent Claim
31 words
A process according to claim 1, wherein said sample is degassed for a period of time sufficient to bring the sample into substantial equilibrium with the initial temperature and vacuum conditions.
Claim 5
Independent Claim
116 words
A method for characterizing materials which evolve gases under vacuum between the temperatures t1 and t2, t1 being less than t2 comprising the steps of: a. subjecting a sample of said material to a high vacuum of at least below 0.1 mm. of Hg. at a temperature of below t1 for a period of time sufficient to remove substantially all of the extraneous adsorbed gases; b. heating said sample while it is maintained under said vacuum to a temperature above t2 at a substantially constant rate whereby gases are evolved; and c. measuring the amount of gas evolved during the heating step (b) at least once and the temperature at which said gas evolved is measured.
Claim 6
Dependent Claim
35 words
A process according to claim 6 wherein the quantity of gas evolved is determined by measuring the gas evolution rate as a function of time over a continuous time interval and integrating the rate-time curve.
Claim 7
Independent Claim
135 words
An apparatus for characterizing materials which evolve gases between the temperatures t1 and t2, t1 being less than t2, comprising: a. sample receiving means; b. means for heating a sample in said sample receiving means from a temperature below t1 to a temperature above t2 at a substantially constant predetermined rate; c. means for measuring the gas flow rate; and d. a first conduit means connecting said flow rate measuring means (c) to said sample receiving means (a) whereby gases Evolved during the heating of said sample are conducted from said sample receiving means to said flow rate measuring means and second conduit means adapted to connect said flow rate measuring means (c) to a high vacuum source whereby gases evolved by desorption from said sample can be withdrawn from the flow rate measuring means.
Claim 8
Dependent Claim
44 words
An apparatus according to claim 8, wherein said means for measuring the gas flow rate comprise (i) a thermal conductivity cell having a heated filament therein and (ii) a reference resistor, said heated filament and said resistor being contained in a Wheatstone bridge circuit.
Claim 9
Dependent Claim
14 words
An apparatus according to claim 9, wherein said reference resistor is a fixed resistor.
Claim 10
Independent Claim
130 words
An apparatus for characterizing materials which evolve gases between the temperatures t1 and t2, t1 being less than t2, comprising: a. sample receiving means; b. means for heating a sample in said sample receiving means from a temperature below t1 to a temperature above t2 at a substantially constant predetermined rate; c. means for measuring the quantity of gas evolved; d. a first conduit means connecting said gas measuring means (c) to said sample receiving means (a) whereby gases evolved during the heating of said sample are conducted from said sample receiving means to said gas measuring means and conduit means adapted to connect said gas measuring means (c) to a high vacuum source whereby gases evolved by desorption from said sample may be withdrawn from said gas measuring means.
Claim 11
Dependent Claim
31 words
An apparatus according to claim 11 wherein said gas measuring means comprises means for measuring gas flow rate and means for integrating the gas flow rate as a function of time.
Claim 12
Independent Claim
111 words
A method for characterizing materials which evolve gases under vacuum between the temperature t1 and t2, t1 being less than t2 comprising the steps of: a. subjecting a sample of said material to a high vacuum of at least below 0.1 mm of Hg. at a temperature of below t1 for a period of time sufficient to remove substantially all of the extraneous absorbed gases; b. heating said sample while it is maintained under said vacuum to a temperature above t2 at a substantially constant predetermined rate, whereby gases are evolved; and c. measuring the rate at which gas is evolved as a function of temperature over a continuous time-temperature interval.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1974-06-28 | 1974-12-28 | 1975-06-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1978-06-28 | 1978-12-28 | 1979-06-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1982-06-28 | 1982-12-28 | 1983-06-29 | $7700.00 | Window Closed / Lapsed |