Patent US4408125A successfully refreshed from Google Patents.
US4408125A
Expired / Lapsed
US
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Modular pyrolysis inlet and method for pyrolyzing compounds for analysis by mass spectrometer
Assignee: University of Utah Research Foundation Inc
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Filing: 1981-07-13
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Granted: 1983-10-04
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Expires: 2001-07-13
Abstract
Abstract A modular pyrolysis inlet apparatus and method for pyrolyzing compounds preparatory to an analysis thereof by a mass spectrometer. The pyrolysis inlet includes a telescopic insertion probe having a ferromagnetic wire bearing the sample to be analyzed, and a reaction chamber mounted to the insertion probe so as to encompass the wire and sample. The insertion probe/reaction chamber assembly is inserted into the pyrolysis inlet apparatus and the voids surrounding the assembly are evacuated. The sample is cooled at a first position within the reaction chamber while a heating mantle preheats the reaction chamber at a second position therein. The telescopic insertion probe/reaction chamber assembly is then inserted further into the pyrolysis inlet, moving the sample to the second heated position within the reaction chamber. At the second position, a high frequency coil is activated to energize and heat the wire, and rapidly pyrolyze the sample thereon. The volatile pyrolysis products escape from the reaction chamber and enter a modular expansion chamber. The volatile pyrolysis products are delayed for a moment within the expansion chamber and then introduced directly into a mass spectrometer for subsequent analysis.
Inventors
- 👤 Hendrik L. C. Meuzelaar
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 22:07
CPC Classifications
H; H01; H01J; H01J49/00; H01J49/02; H01J49/04; G; G01; G01N; G01N1/00; G01N1/02; G01N1/22
Claims Analysis
Total Claims: 46
Claim 1
Independent Claim
138 words
An apparatus for pyrolyzing a sample prior to analysis by a mass spectrometer, comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for preheating at least a portion of the reaction chamber; means for rapidly heating the sample within the preheated portion of the reactant chamber sufficient to pyrolyze the sample, said means for rapidly heating the sample being independent of the preheating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the pyrolyzing apparatus outside of the reaction chamber.
Claim 2
Independent Claim
138 words
An apparatus for pyrolyzing a sample prior to analysis by a mass spectrometer, comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for preheating at least a portion of the reaction chamber; means for rapidly heating the sample within the preheated portion of the reactant chamber sufficient to pyrolyze the sample, said means for rapidly heating the sample being independent of the preheating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the pyrolyzing apparatus outside of the reaction chamber.
Claim 3
Dependent Claim
37 words
An apparatus for pyrolyzing a sample as defined in claim 1 wherein the insertion probe comprises a wire, and wherein the means for rapidly heating the sample is an energy source capable of rapidly heating the wire.
Claim 4
Dependent Claim
56 words
An apparatus for pyrolyzing a sample as defined in claim 2 wherein the means for rapidly heating the sample is a coil capable of emitting electromagnetic energy, and wherein the wire is made of a ferromagnetic material capable of being heated through the absorption of at least a portion of the energy emitted by the coil.
Claim 5
Dependent Claim
26 words
An apparatus for pyrolyzing a sample as defined in claim 3 wherein the reaction chamber preheating means is positioned between the reaction chamber and the coil.
Claim 6
Dependent Claim
42 words
An apparatus for pyrolyzing a sample as defined in claim 4 wherein the reaction chamber preheating means is formed from a single loop of wire such that it does not substantially interfere with the absorption of electromagnetic energy by the ferromagnetic wire.
Claim 7
Dependent Claim
54 words
An apparatus for pyrolyzing a sample as defined in claim 1 wherein the insertion probe is telescopically movable such that the sample may be positioned at a first position outside that portion of the reaction chamber which is preheated and at a second position within that portion of the reaction chamber which is preheated.
Claim 8
Dependent Claim
22 words
An apparatus for pyrolyzing a sample as defined in claim 6 further comprising means for cooling the sample at the first position.
Claim 9
Dependent Claim
38 words
An apparatus for pyrolyzing a sample as defined in claim 1 further comprising an expansion chamber positionned between and providing gaseous communication between the outlet of the reaction chamber and the mass spectrometer during pyrolysis of the sample.
Claim 10
Dependent Claim
19 words
An apparatus for pyrolyzing a sample as defined in claim 8 further comprising means for heating the expansion chamber.
Claim 11
Independent Claim
138 words
An apparatus for pyrolyzing a sample prior to analysis by a mass spectrometer, comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for heating the sample within the reaction chamber sufficient to pyrolyze the sample, the insertion probe being telescopically movable so as to permit first positioning of the sample outside the heating means and second positioning of the sample adjacent the heating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the pyrolyzing apparatus outside of the reaction chamber.
Claim 12
Independent Claim
138 words
An apparatus for pyrolyzing a sample prior to analysis by a mass spectrometer, comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for heating the sample within the reaction chamber sufficient to pyrolyze the sample, the insertion probe being telescopically movable so as to permit first positioning of the sample outside the heating means and second positioning of the sample adjacent the heating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the pyrolyzing apparatus outside of the reaction chamber.
Claim 13
Dependent Claim
22 words
An apparatus for pyrolyzing a sample as defined in claim 10 further comprising means for cooling the sample at the first position.
Claim 14
Dependent Claim
34 words
An apparatus for pyrolyzing a sample as defined in claim 11 wherein the insertion probe comprises a wire, and wherein the heating means further comprises an energy source capable of rapidly heating the wire.
Claim 15
Dependent Claim
52 words
An apparatus for pyrolyzing a sample as defined in claim 12 wherein the energy source is a coil capable of emitting electromagnetic energy, and wherein the wire is made of a ferromagnetic material capable of being heated through the absorption of at least a portion of the energy emitted by the coil.
Claim 16
Dependent Claim
24 words
An apparatus for pyrolyzing a sample as defined in claim 13 wherein the heating means is positionned between the reaction chamber and the coil.
Claim 17
Dependent Claim
34 words
An apparatus for pyrolyzing a sample as defined in claim 14 wherein the heating means has a heating element which does not substantially interfere with the absorption of electromagnetic energy by the ferromagnetic wire.
Claim 18
Dependent Claim
38 words
An apparatus for pyrolyzing a sample as defined in claim 10 further comprising an expansion chamber positioned between and providing gaseous communication between the outlet of the reaction chamber and the mass spectrometer during pyrolysis of the sample.
Claim 19
Dependent Claim
19 words
An apparatus for pyrolyzing a sample as defined in claim 16 further comprising means for heating the expansion chamber.
Claim 20
Independent Claim
186 words
An apparatus for analyzing a sample comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for preheating at least a portion of the reaction chamber, the insertion probe being telescopically movable such that the sample may be positioned at a first position outside that portion of the reaction chamber which is preheated and at a second position within that portion of the reaction chamber which is preheated; means for cooling the sample at the first position; means for rapidly heating the sample sufficient to pyrolyze the sample at the second position within the preheated portion of the reaction chamber, said means for rapidly heating the sample being independent of the preheating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the analyzing apparatus outside of the reaction chamber.
Claim 21
Independent Claim
186 words
An apparatus for analyzing a sample comprising: an insertion probe for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the sample; means for preheating at least a portion of the reaction chamber, the insertion probe being telescopically movable such that the sample may be positioned at a first position outside that portion of the reaction chamber which is preheated and at a second position within that portion of the reaction chamber which is preheated; means for cooling the sample at the first position; means for rapidly heating the sample sufficient to pyrolyze the sample at the second position within the preheated portion of the reaction chamber, said means for rapidly heating the sample being independent of the preheating means; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the analyzing apparatus outside of the reaction chamber.
Claim 22
Dependent Claim
45 words
An apparatus for analyzing a sample as defined in claim 18 further comprising: an expansion chamber positioned between and providing gaseous communication between the outlet of the reaction chamber and the mass spectrometer during pyrolysis of the sample; and means for heating the expansion chamber.
Claim 23
Independent Claim
177 words
An apparatus for analyzing a sample comprising: an insertion probe having a ferromagnetic wire for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the wire and sample; means for creating a partial vacuum within the reaction chamber; means for cooling the sample at a first position within the apparatus; means for heating the reaction chamber at a second position within the apparatus, the insertion probe being telescopically movable so as to permit selective positioning of the sample at the first and second positions; means for transmitting electromagnetic energy to the ferromagnetic wire so as to heat the wire and pyrolyze the sample within the reaction chamber at the second position; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the analyzing apparatus outside of the reaction chamber.
Claim 24
Independent Claim
177 words
An apparatus for analyzing a sample comprising: an insertion probe having a ferromagnetic wire for bearing the sample; a reaction chamber which is mounted to the insertion probe so as to encompass the wire and sample; means for creating a partial vacuum within the reaction chamber; means for cooling the sample at a first position within the apparatus; means for heating the reaction chamber at a second position within the apparatus, the insertion probe being telescopically movable so as to permit selective positioning of the sample at the first and second positions; means for transmitting electromagnetic energy to the ferromagnetic wire so as to heat the wire and pyrolyze the sample within the reaction chamber at the second position; and an outlet formed in the reaction chamber to allow passage of the pyrolyzed sample into a mass spectrometer positioned adjacent the reaction chamber, said outlet being positioned so as to direct the pyrolyzed sample into the mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions of the analyzing apparatus outside of the reaction chamber.
Claim 25
Dependent Claim
37 words
An apparatus for pyrolyzing a sample as defined in claim 20 further comprising an expansion chamber removably positioned between the outlet of the reaction chamber and the mass spectrometer when the sample is at the second position.
Claim 26
Independent Claim
98 words
A method for analyzing a sample comprising the steps of: preheating at least a portion of a reaction chamber; introducing the sample into the preheated portion of the reaction chamber; rapidly heating the sample within the preheated portion of the reaction chamber so as to pyrolyze the sample, the rapid heating of the sample being achieved independently of the preheating of the reaction chamber; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 27
Independent Claim
98 words
A method for analyzing a sample comprising the steps of: preheating at least a portion of a reaction chamber; introducing the sample into the preheated portion of the reaction chamber; rapidly heating the sample within the preheated portion of the reaction chamber so as to pyrolyze the sample, the rapid heating of the sample being achieved independently of the preheating of the reaction chamber; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 28
Dependent Claim
49 words
A method for analyzing a sample as defined in claim 22 further comprising the step of cooling a portion of the reaction chamber and positioning the sample within the cool portion of the reaction chamber prior to introduction of the sample into the preheated portion of the reaction chamber.
Claim 29
Dependent Claim
26 words
A method for analyzing a sample as defined in claim 22 further comprising the step of delaying passage of the pyrolyzed sample into the mass spectrometer.
Claim 30
Independent Claim
136 words
A method for analyzing a sample comprising the steps of: securing a wire to the end of an insertion probe, the insertion probe being telescopically movable so as to permit variable positioning of the wire; placing the sample on the wire; introducing the wire and sample into a reaction chamber at a first position therein and securing the reaction chamber to the insertion probe; cooling the sample at the first position; moving the insertion probe so as to introduce the sample at a second position within the reaction chamber; heating the sample at the second position so as to pyrolyze the sample; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 31
Independent Claim
136 words
A method for analyzing a sample comprising the steps of: securing a wire to the end of an insertion probe, the insertion probe being telescopically movable so as to permit variable positioning of the wire; placing the sample on the wire; introducing the wire and sample into a reaction chamber at a first position therein and securing the reaction chamber to the insertion probe; cooling the sample at the first position; moving the insertion probe so as to introduce the sample at a second position within the reaction chamber; heating the sample at the second position so as to pyrolyze the sample; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 32
Dependent Claim
39 words
A method for analyzing a sample as defined in claim 25 further comprising the step of preheating a portion of the reaction chamber adjacent the second position of the sample prior to moving the sample to the second position.
Claim 33
Dependent Claim
29 words
A method for analyzing a sample as defined in claim 25 further comprising the step of preventing gaseous components of the pyrolyzed sample from condensing in the reaction chamber.
Claim 34
Dependent Claim
26 words
A method for analyzing a sample as defined in claim 25 further comprising the step of delaying passage of the pyrolyzed sample into the mass spectrometer.
Claim 35
Independent Claim
194 words
A method for analyzing a sample comprising the steps of: securing a wire capable of being rapidly heated to the end of an insertion probe, the insertion probe being telescopically movable so as to permit variable positioning of the wire; placing the sample on the wire; introducing the wire and sample into a reaction chamber at a first position therein and securing the reaction chamber to the insertion probe; cooling a first portion of the reaction chamber at the first position; preheating a second portion of the reaction chamber at a second position therein; moving the insertion probe so as to introduce the wire and sample into the preheated portion of the reaction chamber at the second position; rapidly heating the wire within the preheated portion of the reaction chamber at the second position so as to pyrolyze the sample, the rapid heating of the sample being achieved independently of the preheating of the second portion of the reaction chamber; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 36
Independent Claim
194 words
A method for analyzing a sample comprising the steps of: securing a wire capable of being rapidly heated to the end of an insertion probe, the insertion probe being telescopically movable so as to permit variable positioning of the wire; placing the sample on the wire; introducing the wire and sample into a reaction chamber at a first position therein and securing the reaction chamber to the insertion probe; cooling a first portion of the reaction chamber at the first position; preheating a second portion of the reaction chamber at a second position therein; moving the insertion probe so as to introduce the wire and sample into the preheated portion of the reaction chamber at the second position; rapidly heating the wire within the preheated portion of the reaction chamber at the second position so as to pyrolyze the sample, the rapid heating of the sample being achieved independently of the preheating of the second portion of the reaction chamber; and allowing passage of the pyrolyzed sample from the reaction chamber into a mass spectrometer while substantially prohibiting passage of the pyrolyzed sample into regions outside of the reaction chamber and the mass spectrometer.
Claim 37
Dependent Claim
17 words
An apparatus for pyrolyzing a sample as defined in claim 1 wherein the reaction chamber is replaceable.
Claim 38
Dependent Claim
16 words
An apparatus for pyrolyzing a sample as defined in claim 2 wherein the wire is replaceable.
Claim 39
Dependent Claim
66 words
An apparatus for pyrolyzing a sample as defined in claim 1 wherein the preheating means is capable of preheating the portion of the reaction chamber to be preheated to a temperature of up to about 500° C. and wherein the means for rapidly heating the sample is capable of heating the sample to a temperature within the range of about 358° C. to about 1128° C.
Claim 40
Dependent Claim
17 words
An apparatus for pyrolyzing a sample as defined in claim 10 wherein the reaction chamber is replaceable.
Claim 41
Dependent Claim
16 words
An apparatus for pyrolyzing a sample as defined in claim 12 wherein the wire is replaceable.
Claim 42
Dependent Claim
21 words
An apparatus for analyzing a sample as defined in claim 20 wherein the ferromagnetic wire and the reaction chamber are replaceable.
Claim 43
Dependent Claim
40 words
A method for analyzing a sample as defined in claim 22 further comprising the step of replacing the reaction chamber after pyrolysis of the sample with a clean reaction chamber so as to provide a clean environment for subsequent analyses.
Claim 44
Dependent Claim
58 words
A method for analyzing a sample as defined in claim 22 wherein the preheated portion of the reaction chamber is at a temperature of up to about 500° C. and wherein the sample is rapidly heated to a temperature within the range of about 358° C. to about 1128° C. within the preheated portion of the reaction chamber.
Claim 45
Dependent Claim
47 words
A method for analyzing a sample as defined in claim 25 further comprising the step of replacing the wire and the reaction chamber after pyrolysis of the sample with a clean wire and a clean reaction chamber so as to provide a clean environment for subsequent analyses.
Claim 46
Dependent Claim
47 words
A method for analyzing a sample as defined in claim 29 further comprising the step of replacing the wire and the reaction chamber after pyrolysis of the sample with a clean wire and a clean reaction chamber so as to provide a clean environment for subsequent analyses.
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1986-10-03 | 1987-04-04 | 1987-10-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-10-03 | 1991-04-04 | 1991-10-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-10-03 | 1995-04-04 | 1995-10-04 | $7700.00 | Window Closed / Lapsed |