US4517461A
Expired / Lapsed
US
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Carbon isotope analysis of hydrocarbons
Assignee: Phillips Petroleum Co
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Filing: 1982-11-29
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Granted: 1985-05-14
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Expires: 2002-11-29
Abstract
Abstract Method and apparatus are provided for analysis of a sample of matter for at least one isotopic constituent of the sample. The method involves introduction of a sample containing an isotope of interest into an analytical detector operative to convert the sample into a product analyzable by a mass spectrometer and to detect a property of the sample representative of the quantity of at least one of its constituents, and passing the conversion product from the detector to a mass spectrometer operative to detect the isotopic ratio of interest. The method optionally includes passing the sample or a source material through a chromatograph column for separation into suitable fractions. The apparatus includes an appropriate analytical detector and a mass spectrometer with optional chromatography column. The method and instrument are particularly suited for analysis of oil-related samples such as crude oil fractions, natural gas, soil gas and oil shale as a tool in oil prospecting.
Inventors
- 👤 John A. Crandall
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 01:33
CPC Classifications
B; B01; B01D; B01D59/00; B01D59/44; G; G01; G01N; G01N30/00; G01N30/02; G01N2030/022; G01N2030/025; G01N30/62; G01N30/72; G01N30/7206
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
128 words
A method comprising: introducing a sample of matter containing an isotope of interest selected from isotopes of carbon and sulfur into an analytical detector selected from a flame ionization detector and a flame photometric detector operative to combust the sample and to detect a property representative of the presence of carbon or sulfur of the sample or a combustion product thereof, and producing combustion product comprising at least one of carbon dioxide and sulfur dioxide containing the isotope of interest; and passing at least the isotope of interest portion of the combustion product to a mass spectrometer operative to make a quantitative isotopic analysis of the isotope of interest and producing an output from the mass spectrometer representative of the quantitative isotopic analysis of the isotope of interest.
Claim 2
Independent Claim
128 words
A method comprising: introducing a sample of matter containing an isotope of interest selected from isotopes of carbon and sulfur into an analytical detector selected from a flame ionization detector and a flame photometric detector operative to combust the sample and to detect a property representative of the presence of carbon or sulfur of the sample or a combustion product thereof, and producing combustion product comprising at least one of carbon dioxide and sulfur dioxide containing the isotope of interest; and passing at least the isotope of interest portion of the combustion product to a mass spectrometer operative to make a quantitative isotopic analysis of the isotope of interest and producing an output from the mass spectrometer representative of the quantitative isotopic analysis of the isotope of interest.
Claim 3
Dependent Claim
36 words
The method of claim 1 in which the analytical detector is a flame ionization detector operative to detect a property of the sample representative of its content of a substance selected from methane, ethane and propane.
Claim 4
Dependent Claim
23 words
The method of claim 1 in which the sample is selected from natural gas, petroleum, soil gas, shale, coal and constituents of these.
Claim 5
Dependent Claim
37 words
The method of claim 1 which further comprises passing a gaseous mixture through a gas chromatography column and separating the mixture into at least two constituents, one of which is the sample containing the isotope of interest.
Claim 6
Dependent Claim
23 words
The method of claim 1 in which the analytical detector is a flame ionization detector and the isotope of interest is carbon 13.
Claim 7
Dependent Claim
23 words
The method of claim 1 in which the analytical detector is a flame photometric detector and the isotope of interest is sulfur 34.
Claim 8
Dependent Claim
23 words
The method of claim 6 which further comprises determining from the isotopic analysis a property of the sample related to its geological history.
Claim 9
Dependent Claim
24 words
The method of claim 1 in which the sample of matter has a volume of about 1 cc to about 25 cc at STP.
Claim 10
Dependent Claim
17 words
The method of claim 8 in which the sample is a pyrolysis product of a solid material.
Claim 11
Dependent Claim
37 words
The method of claim 8 which further comprises passing a gaseous mixture through a gas chromatography column and separating the mixture into at least two constituents, one of which is the sample containing the isotope of interest.
Claim 12
Dependent Claim
47 words
The method of claim 10 in which the sample is passed to the analytical detector in a carrier gas and the combustion product containing the isotope of interest is concentrated with respect to the carrier gas prior to introduction of the combustion product into the mass spectrometer.
Claim 13
Dependent Claim
108 words
Apparatus for analyzing a sample of matter for an isotope of interest selected from isotopes of carbon and sulfur, the apparatus comprising: an analytical detector selected from a flame ionization detector and a flame photometric detector operative to convert a sample into a product comprising the isotope of interest and to detect a property representative of the presence of carbon or sulfur of an amount of an introduced material within the range of about 1 cc to about 25 cc at STP; a mass spectrometer having an inlet in flow communication with the analytical detector and operative to make a quantitative isotopic analysis of the isotope of interest.
Claim 14
Dependent Claim
108 words
Apparatus for analyzing a sample of matter for an isotope of interest selected from isotopes of carbon and sulfur, the apparatus comprising: an analytical detector selected from a flame ionization detector and a flame photometric detector operative to convert a sample into a product comprising the isotope of interest and to detect a property representative of the presence of carbon or sulfur of an amount of an introduced material within the range of about 1 cc to about 25 cc at STP; a mass spectrometer having an inlet in flow communication with the analytical detector and operative to make a quantitative isotopic analysis of the isotope of interest.
Claim 15
Dependent Claim
16 words
The apparatus of claim 12 in which the mass spectrometer is an isotope ratio mass spectrometer.
Claim 16
Dependent Claim
21 words
The apparatus of claim 13 which further comprises a chromatography column having an outlet in flow communication with the analytical detector.
Claim 17
Dependent Claim
43 words
The apparatus of claim 12 in which the analytical detector is a flame ionization detector having an outlet for combustion products in flow communication with the inlet of the mass spectrometer via means to concentrate the combustion products relative to a carrier gas.
Claim 18
Dependent Claim
17 words
The apparatus of claim 15 in which the combustion product concentration means is a glass jet separator.
Claim 19
Dependent Claim
20 words
The apparatus of claim 14 which further comprises means to remove water vapor from combustion products of the analytical detector.
Claim 20
Dependent Claim
112 words
The apparatus of claim 12 which comprises: a gas chromatography column having an inlet and an outlet; means to introduce a gaseous sample in a quantity of about 1 cc to about 25 cc into the inlet of the gas chromatography column; a flame ionization detector having a sample inlet and a combustion product outlet, the inlet being in flow communication with the outlet of the gas chromatography column; an isotope ratio mass spectrometer having an inlet in flow communication with the outlet of the flame ionization detector; and means to remove water from a gas flowing from the outlet of the flame ionization detector to the inlet of the mass spectrometer.
Claim 21
Dependent Claim
32 words
The apparatus of claim 18 further comprising means for carrier gas introduction and means for reduction of carrier gas concentration between the outlet of the flame ionization detector and the mass spectrometer.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-05-13 | 1988-11-12 | 1989-05-14 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-05-13 | 1992-11-12 | 1993-05-14 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-05-13 | 1996-11-12 | 1997-05-14 | $7700.00 | Window Closed / Lapsed |