Method and system for chemical and physical characterization of complex samples

• US 8,413,484 B2
• Filed: 06/29/2007
• Issued: 04/09/2013
• 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:
  US11/819,861
• Publication Number:
  US 20080296487A1
• Time in Patent Office: 2,111 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 30/78 using more than one detector
• 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 hydrocarbon type 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 ion detector (FID);

a mass spectrometer; and

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

wherein the divider is configured to prevent molecular discrimination within the constituents of the sample.

2. The system according to claim 1, wherein the system further comprises:

a data processor for acquiring and processing data.

3. The system according to claim 2, wherein the data processor is configured to process the data by combining detection information from the flame ion detector and the mass spectrometer.

4. The system according to claim 2, wherein the data processor processes the data by combining detection information from the flame ion detector and the mass spectrometer via algorithms that allow the superimposition of masses at various intervals to extract a composition of the sample.

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

6. The system according to claim 1, wherein the column is a wall coated capillary column.

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

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

9. 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.

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

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

12. The system according to claim 1, wherein a controller controls a pressure of the sample to prevent molecular discrimination within the constituents of the sample.

13. The system according to claim 1, wherein the sample is heated to an appropriate temperature to prevent molecular discrimination.

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

15. The system of claim 1, wherein molecular discrimination is prevented by:

a first portion of the constituents that is sent to the mass spectrometer and a second portion of the constituents that is sent to the flame ion detector being approximately equal; and

an integrity of the constituents is preserved.

16. 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 delivery to a flame ion detector and a mass spectrometer;

detecting characteristics of the constituents of the sample via the flame ion detector; and

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

wherein dividing the constituents of the sample comprises preventing molecular discrimination within the constituents of the sample.

17. The method of claim 16, further comprising:

acquiring and processing data from the detected characteristics obtained from the flame ion detector and the mass spectrometer.

18. The method of claim 17, wherein acquiring and processing the data includes:

combining detection information from the flame ion detector and the mass spectrometer.

19. The method according to claim 17, wherein acquiring and processing data is performed via algorithms that allow the superimposition of masses at various intervals to extract a composition of the sample.

20. The method of claim 16, wherein the sample is injected with a temperature programmable injector.

21. The method of claim 16, wherein the sample is injected into wall coated capillary column.

22. The method of claim 16, wherein detecting characteristics of the constituents of the sample via the flame ion detector occurs in a simulated distillation mode.

23. The method of claim 16, wherein the divider approximately equally divides the constituents of the sample that are exiting the column.

24. The method of claim 16, wherein the flowing gas is helium, and the method further comprising:

configuring the gas chromatograph to maintain the flowing gas at a constant flux of about 12 mL/minute.

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

26. The method of claim 16, wherein the sample is a fraction of crude oil.

27. The method according to claim 16, wherein a controller controls a pressure of the sample to prevent molecular discrimination within the constituents of the sample.

28. The method according to claim 16, wherein the sample is heated to an appropriate temperature to prevent molecular discrimination.

29. The method of to claim 16, wherein the flowing gas is hydrogen, and the method further comprising:

configuring the gas chromatograph to maintain the flowing gas at a constant flux of about 12 mL/minute.

30. The method of claim 16, wherein preventing molecular discrimination within the constituents of the sample comprises:

having a first portion of the constituents that is sent to the mass spectrometer and a second portion of the constituents that is sent to the flame ion detector be approximately equal; and

preserving an integrity of the constituents.