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US4757023A
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Method and equipment for the simulated distillation by means of gas chromatography with non vaporizing direct injection
Assignee: Fisons Instruments SpA
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Filing: 1985-12-19
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Granted: 1988-07-12
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Expires: 2005-12-19
Abstract
Abstract The invention concerns a method and an equipment for the simulated distillation, by means of gas chromatography, of petroleum products, capable of characterizing also high boiling products, exceeding C55, over 600 C TBP. A chromatograph is used with a capillary column having a length less than or equal to 10 m, containing an immobilized non polar polydimethylsilicon gum stationary phase with a film thickness less than or equal to 0.2 μm. The sample is introduced through a non vaporizing direct cold on-column injection and the eluted sample is detected by means of a FID detector. The column oven is operated in temperature programming conditions up to temperatures exceeding 400 (up to 430-450 C.).
Inventors
- 👤 Sorin Trestianu
- 👤 Fausto Munari
- 👤 Carlo Saravalle
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 05:24
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/88; G01N2030/022; G01N2030/025; G01N2030/8809; G01N2030/884; G01N2030/8854; G01N33/00; G01N33/26; G01N33/28
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
248 words
A method of the simulated distillation of petroleum products utilizing apparatus adapted for chromatographic analysis including a capillary column wherein said capillary column has an inner diameter ranging between 0.2 and 0.6 mm and a length between 1 and 10 m, said capillary column having therein a thin film stationary phase less than or equal to 0.2 μm, said capillary column having a first end and a second end and having associated with said first end of said capillary column a direct nonvaporizing cold on-column injector and an oven in which said capillary column is housed, said oven being programmable to reach temperatures over 400° C. at a speed equal to at least 5° C. per minute and wherein said apparatus has a flame ionization detector connected to said second end of said column, said method comprising the steps of: (a) injecting into said column utilizing said direct cold on-column injector an appropriately diluted sample of a sample petroleum product; (b) performing a gas chromatographic analysis on said sample petroleum product using said apparatus at a preprogrammed temperature having a temperature end point greater than 400° C.; (c) converting said time axis of said chromatogram obtained from said gas chromatographic analysis of said sample petroleum product into a boiling point axis by using a standard calibration mixture which generates a standard curve; and (d) integrating in slices the surface between the sample elution curve and the chromatogram base line to obtain a simulated distillation boiling point distribution curve.
Claim 2
Independent Claim
248 words
A method of the simulated distillation of petroleum products utilizing apparatus adapted for chromatographic analysis including a capillary column wherein said capillary column has an inner diameter ranging between 0.2 and 0.6 mm and a length between 1 and 10 m, said capillary column having therein a thin film stationary phase less than or equal to 0.2 μm, said capillary column having a first end and a second end and having associated with said first end of said capillary column a direct nonvaporizing cold on-column injector and an oven in which said capillary column is housed, said oven being programmable to reach temperatures over 400° C. at a speed equal to at least 5° C. per minute and wherein said apparatus has a flame ionization detector connected to said second end of said column, said method comprising the steps of: (a) injecting into said column utilizing said direct cold on-column injector an appropriately diluted sample of a sample petroleum product; (b) performing a gas chromatographic analysis on said sample petroleum product using said apparatus at a preprogrammed temperature having a temperature end point greater than 400° C.; (c) converting said time axis of said chromatogram obtained from said gas chromatographic analysis of said sample petroleum product into a boiling point axis by using a standard calibration mixture which generates a standard curve; and (d) integrating in slices the surface between the sample elution curve and the chromatogram base line to obtain a simulated distillation boiling point distribution curve.
Claim 3
Dependent Claim
14 words
The method according to claim 1 including feeding a carrier gas into said column.
Claim 4
Dependent Claim
14 words
The method according to claim 1 wherein said carrier gas is hydrogen or helium.
Claim 5
Dependent Claim
41 words
The method according to claim 2 wherein said feeding of said carrier gas into said column is carried out by feeding said carrier gas at a constant pressure during said injecting and at a constant flow during said gas chromatographic analysis.
Claim 6
Dependent Claim
34 words
The method according to claim 1 wherein the step of obtaining a standard curve comprises extrapolating a curve of boiling points of n-alkanes with respect to the number of carbon atoms of said n-alkanes.
Claim 7
Dependent Claim
19 words
The method according to claim 1 wherein said capillary column is formed of fused silica with a polyimide coating.
Claim 8
Dependent Claim
22 words
The method according to claim 6 comprising the step of feeding an inert gas into said oven prior to said chromatographic analysis.
Claim 9
Dependent Claim
20 words
The method according to claim 1 wherein said standard calibration mixture has a molecular weight from about 500 to 150.
Claim 10
Dependent Claim
33 words
The method according to claim 1 comprising the further step of performing a deasphaltation step on said sample petroleum product prior to injecting said petroleum product sample into said column for chromatographic analysis.
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) | 1991-07-12 | 1992-01-11 | 1992-07-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-07-12 | 1996-01-11 | 1996-07-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-07-12 | 2000-01-11 | 2000-07-12 | $7700.00 | Window Closed / Lapsed |