Method and system for chemical and physical characterization of complex samples

• US 7,509,837 B2
• Filed: 10/18/2006
• Issued: 03/31/2009
• Est. Priority Date: 10/18/2005
• Status: Expired due to Fees

• Current Assignee: Separation Systems Inc.
• Original Assignee: Separation Systems Inc.
• Inventors: Lubkowitz, Joaquin A., Mendez, Aaron, Meneghini, Roberto I.
• Primary Examiner(s): LARKIN, DANIEL SEAN
• Application Number:
  US11/582,558
• Publication Number:
  US 20070181798A1
• Time in Patent Office: 895 Days
• Field of Search: 73/233.5, 73/233.7, 73/233.9, 73/234, 73/234.1
• US Class Current: 73/23.35
• CPC Class Codes: G01N 2030/8854 involving hydrocarbons
• CPC Class Codes: G01N 30/68 Flame ionisation detectors
• CPC Class Codes: G01N 30/7206 interfaced to gas chromatograph interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04
• CPC Class Codes: G01N 30/8675 Evaluation, i.e. decoding of the signal into analytical information for analysis of specific compounds see also G01N30/88 and subgroups of G01N33/00; chemical libraries per se C40B
• CPC Class Codes: G01N 30/8682 Group type analysis, e.g. of components having structural properties in common
• CPC Class Codes: G01N 30/8686 Fingerprinting, e.g. without prior knowledge of the sample components
• CPC Class Codes: G01N 33/28 Oils , i.e. hydrocarbon liquidsgaseous fuels G01N33/225; edible oils or edible fats G01N33/03

Abstract

A method and system for rapid determination of a composition, such as crude oils and fractions thereof, and s obtaining the information necessary to assess the yield of commercially valuable fuel and lube oil fractions in a single process, variations of the method and system use Gas Chromatography—FID/Mass Spectrometry and other features, including an auto sampler, a wall coated capillary column, a temperature programmable injector, and a data processing system for compiling and processing the experimental data. The system and method further include a computer system with application software or other processing mechanism and optionally a communication network. One variation provides a graphical user interface for the entry of data and for displaying information, such as in a graphical manner, to show the relationship of various determined outputs and results.

Claims

1. A system for analyzing complex samples, the system comprising:

a gas chromatograph including an injector and a column, wherein the injector is configured to insert a sample along with a flowing gas into the column;

a flame ionization detector (FID);

a mass spectrometer;

a divider configured to divide constituents of the sample that are exiting the column for contemporaneous delivery to the flame ionization detector and the mass spectrometer; and

a data processor for acquiring and processing data obtained from the flame ionization detector and the mass spectrometer,

wherein the data processor is configured to process the data by combining detection information from the flame ionization detector and the mass spectrometer,

wherein the data processor further provides detailed composition information for the sample and the sample comprises hydrocarbon,

wherein the detailed composition information comprises a quantitative percent mass yield as a function of a boiling point of the hydrocarbon components of the sample.

2. The system according to claim 1, wherein the injector is a temperature programmable injector.

4. The system according to claim 1, wherein the FID is in a simulated distillation mode.

5. The system according to claim 1, wherein the divider is configured to equally divide the constituents of the sample that are exiting the column.

6. The system according to claim 1, wherein the gas used in the gas chromatograph is helium, and wherein the gas chromatograph is configured to maintain the gas at a constant flux of about 12 mL/minute.

7. The system according to claim 1 wherein the injector is configured to inject a sample of dense material.

8. The system according to claim 7, wherein the dense material includes crude oil.

9. The system according to claim 1, wherein the injector is configured to inject a sample of a fraction of crude oil.

3. The system according to claim I wherein the column is a wall coated capillary column.

10. A method of analyzing a complex sample, the method including:

injecting a sample with an injector into a column of a gas chromatograph along with a flowing gas;

separating constituents of the sample within the column of the gas chromatograph;

moving the constituents of the sample out of the column with the flowing gas;

dividing the constituents of the sample that are exiting the column for contemporaneous delivery to a flame ionization detector and a mass spectrometer;

detecting characteristics of the constituents of the sample via the flame ionization detector;

detecting characteristics of the constituents of the sample via the mass spectrometer;

acquiring and processing data from the detected characteristics obtained from the flame ionization detector and the mass; and

combining detection information from the flame ionization detector and the mass spectrometer,

wherein the acquiring and processing data further comprises providing detailed composition information for the sample,

wherein the sample comprise hydrocarbon,

wherein the detailed composition information comprises a quantitative percent mass yield as a function of a boiling point of the hydrocarbon components of the sample.

11. The method of claim 10, wherein the sample is injected with a temperature programmable injector.

12. The method of claim 10, wherein the sample is injected into a wall coated capillary column.

13. The method of claim 10, wherein detecting characteristics of the constituents of the sample via the flame ionization detector occurs in a simulated distillation mode.

14. The method of claim 10, wherein the divider approximately equally divides the constituents of the sample that are exiting the column.

15. The method of claim 10, wherein the flowing gas is helium, and the method further comprising:

configuring the gas chromatograph to maintain the flowing gas at a constant flux.

16. The method of claim 10, wherein the sample is crude oil.

17. The method of claim 10, wherein the sample is a fraction of crude oil.