High pressure and high temperature chromatography

• US 8,028,562 B2
• Filed: 12/17/2007
• Issued: 10/04/2011
• Est. Priority Date: 12/17/2007
• Status: Active Grant

• Current Assignee: Schlumberger Technology Corporation (SLB)
• Original Assignee: Schlumberger Technology Corporation (SLB)
• Inventors: Paso, Kristofer Gunnar, Shah, Jagdish, Bostrom, Neil William, Raghuraman, Bhavani, Zhdaneev, Oleg
• Primary Examiner(s): Williams; Hezron E
• Assistant Examiner(s): DEVITO, ALEX T
• Application Number:
  US11/958,049
• Publication Number:
  US 20090151426A1
• Time in Patent Office: 1,387 Days
• Field of Search: None
• US Class Current: 73/23.35
• CPC Class Codes: G01N 2030/8809 analysis specially adapted for the sample
• CPC Class Codes: G01N 2030/8854 involving hydrocarbons
• CPC Class Codes: G01N 30/22 in high pressure liquid systems
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/88 Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
• CPC Class Codes: G01N 33/2823 Raw oil, drilling fluid or polyphasic mixtures

Abstract

Methods and related systems are described for high pressure chromatographic analysis. The described system includes a flowpath adapted to flow a mobile phase and the sample at high pressures, an injector adapted to inject the fluid sample into a flowpath, a separation column adapted to operate at high pressures for separating various components, a detector and a processor that calculates the amount of at least one component of the fluid sample. The system can operate a pressures above 20 atm or even 100 atm, and temperatures above about 100 degrees Celsius. The system can deployed in a wellbore in a subterranean rock formation, and include fluid collection system for obtaining the fluid sample downhole. The system can also be located close to a wellhead and includes a tap in fluid communication with a surface flowline carrying produced fluids and the injector.

Claims

1. A system for high pressure gas chromatographic analysis of a fluid sample, the system comprising:

a pressure balanced tool housing constructed and adapted for deployment in a wellbore in a subterranean rock formation;

a fluid collection system for obtaining the fluid sample downhole;

a mobile gas phase of a controllable mobile gas phase source in communication with a controllable expander injector coordinately maintains the fluid sample at pressures similar to a pressure of the subterranean rock formation from which the fluid sample was collected;

a flowpath adapted to flow the mobile gas phase and the fluid sample at pressures above 20 atmospheres and at ambient temperatures above 100 degrees Celsius and the controllable expander injector is adapted to convert the fluid sample into a gas phase to inject the fluid sample into the flowpath as a gas;

a separation column adapted to operate at high pressures, forming part of the flowpath downstream of the controllable expander injector, for separating a plurality of components within the fluid sample;

a detector located downstream of the separation column, measuring at least one property of the gas, thereby generating measurement data representing properties of at least one component of the fluid sample, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within the tool housing and adapted to operate at pressures approximate to the incoming downhole pressure of the fluid sample from which the fluid sample was collected; and

a processor adapted to calculate from the measurement data a value relating to the amount of at least one component of the fluid sample.

2. The system according to claim 1, wherein the system is adapted to operate at pressures above about 20 atmospheres.

3. The system according to claim 1, wherein the system is adapted to operate at pressures above about 100 atmospheres.

4. The system according to claim 1, wherein the system is adapted to operate at ambient temperatures above 100 degrees Celsius.

5. The system according to claim 1, further comprising:

a heating and cooling device that is capable of providing variable temperatures to the separation column.

6. The system according to claim 1, further comprising a tap in fluid communication with a surface flowline carrying produced fluids and said controllable expander injector.

7. The system according to claim 6, wherein the system is in close proximity a wellhead of the wellbore.

8. The system according to claim 7, wherein the tap is located on the surface flowline prior to any significant pressure drop in the produced fluids after the wellhead.

9. The system according to claim 1, further comprising a container adapted to contain the fluid sample at high pressure, and being in fluid communication with the controllable expander injector.

10. The system according to claim 1, wherein the separation column is not a packed column.

11. The system according to claim 1, wherein the calculated value relating to the at least one component is selected from a group consisting of:

mass concentration of a component, volume concentration of a component, and ratio of components.

12. A method for high pressure gas chromatographic analysis of a fluid sample containing a plurality of components, the method comprising the steps of:

obtaining the fluid sample with a fluid collection system utilizing a pressure balanced tool housing in a wellbore in a subterranean rock formation;

using a mobile gas phase of a controllable mobile gas phase source in communication with a controllable expander injector that coordinately maintains the fluid sample as pressure similar to a pressure of the subterranean rock formation from which the fluid sample was collected;

flowing the injected fluid sample through a separation column;

detecting a property of the fluid sample in the flow path with a detector thereby generating measurement data; and

calculating from the measurement data a value relating to the amount of at least one component of the fluid sample, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within a tool housing and adapted to operate at pressures approximate to the incoming downhole pressure of the fluid sample from which the fluid sample was collected.

13. The method according to claim 12, wherein the flowpath is adapted to operate at pressures above about 20 atmospheres.

14. The method according to claim 12, wherein the flowpath is adapted to operate at pressures above about 100 atmospheres.

15. The method according to claim 12, wherein the flowpath is adapted to operate at ambient temperatures above 100 degrees Celsius.

16. The method according to claim 12, further comprising the step of collecting the fluid sample downhole wherein said steps of injecting, flowing and detecting are carried out downhole.

17. The method according to claim 12, wherein collecting the fluid sample and said steps of injecting, flowing and detecting are carried out in close proximity to the wellbore.

18. The method according to claim 17, wherein said step of collecting the fluid sample is carried out at a location on a surface flowline prior to any significant pressure drop in produced fluids from the wellbore.

19. The method according to claim 12, further comprising the steps of:

containing the fluid sample at high pressure within a container; and

flowing the fluid sample from the container to the controllable expander injector.

20. The method according to claim 12, wherein the separation column is not a packed column.

21. The method according to claim 12, wherein the calculated value relating to the at least one component is selected from a group consisting of:

mass concentration of a component, volume concentration of a component, or ratio of components.

22. A system of for high pressure chromatographic analysis of a fluid sample, the system comprising:

a pressure balanced tool housing constructed and adapted for deployment in a wellbore in a subterranean rock formation;

a fluid collection system for obtaining the fluid sample downhole;

a mobile gas phase of a controllable mobile gas phase source in communication with a controllable expander injector coordinately maintains the fluid sample at pressures similar to a pressure of the subterranean rock formation from which the fluid sample was collected;

a flowpath adapted to flow a mobile phase and the fluid sample at pressures above about 20 atmospheres;

controllable expander injector adapted to convert the fluid sample into a gas phase to inject the fluid sample into a flowpath as a gas;

a separation column adapted to operate at pressures above about 20 atmospheres, forming part of the flowpath downstream of the controllable expander injector, for separating a plurality of components within the fluid sample, wherein the separation column is not a packed column; and

a detector located downstream of the separation column, the detector adapted to measure properties of the fluid sample, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within the tool housing, and adapted to operate at pressures approximate to the incoming pressure of the fluid sample from which the fluid sample was collected.

23. The system according to claim 22, further comprising a processing system adapted calculate from measurements made by the detector a value relating to the amount of at least one component of the fluid sample.

24. The system according to claim 23, wherein the calculated value relating to the at least one component is selected from a group consisting of:

mass concentration of a component, volume concentration of a component, or ratio of components.

25. The system according to claim 22, wherein the system is adapted to operate at pressures above about 100 atmospheres.

26. The system according to claim 22, wherein the system is adapted to operate at ambient temperatures above 100 degrees Celsius.

27. The system according to claim 22, further comprising:

a tool housing constructed and adapted to be deployed in a wellbore in a subterranean rock formation; and

a fluid collection system for obtaining the fluid sample downhole, wherein the injector, column and detector are housed within the tool housing and adapted to operate under downhole conditions.

28. The system according to claim 22, further comprising a tap in fluid communication with a surface flowline carrying produced fluids and said controllable expander injector.

29. A system for downhole chromatographic analysis of a fluid sample, the system comprising:

a pressure balanced tool housing constructed and adapted to be deployed in a wellbore in a subterranean rock formation;

a fluid collection system for obtaining the fluid sample downhole;

a mobile gas phase of a controllable mobile gas phase source in communication with a controllable expander injector coordinately maintains the fluid sample at pressures similar to a pressure of the subterranean rock formation from which the fluid sample was collected;

a flowpath adapted to flow the mobile gas phase and the fluid sample at pressures above 20 atmospheres and at ambient temperatures above 100 degrees Celsius, and the controllable expander injector is adapted to convert the fluid sample into a gas phase to inject the fluid sample into the flowpath as a gas;

a separation column forming part of the flowpath downstream of the controllable expander injector, for separating a plurality of components within the fluid sample; and

a detector housed within the separation column located downstream of the separation column, the detector adapted to measure properties of the fluid sample, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within the tool housing and adapted to operate at pressures approximate to the incoming downhole pressure of the fluid sample from which the fluid sample was collected.

30. The system according to claim 29, wherein the tool housing forms part of a wireline toolstring adapted to be deployed in the wellbore via a wireline cable.

31. The system according to claim 29, further comprising a processing system adapted calculate from measurements made by the detector a value relating to the amount of at least one component of the downhole fluid sample.

32. The system according to claim 31, wherein the calculated value relating to the at least one component is selected from a group consisting of:

mass concentration of a component, volume concentration of a component, or ratio of components.

33. The system according to claim 31, wherein the processing system is adapted to remain on the surface while the tool housing is deployed in the wellbore, and the processing system is in communication with the tool housing through at least a communication cable.

34. The system according to claim 29, wherein the system is adapted to operate at pressures above about 20 atmospheres.

35. The system according to claim 29, wherein the system is adapted to operate at ambient temperatures above 100 degrees Celsius.

36. A system for chromatographic analysis of a fluid sample at high ambient temperatures, the system comprising:

a pressure balanced tool housing constructed and adapted to be deployed in a wellbore in a subterranean rock formation;

a fluid collection system for obtaining the fluid sample downhole;

a mobile gas phase of a controllable mobile gas phase source in communication with a controllable expander injector coordinately maintains the fluid sample at pressures similar to a pressure of the subterranean rock formation from which the fluid sample was collected;

a flowpath adapted to flow the mobile gas phase and the fluid sample at pressures above 20 atmospheres and the controllable expander injector is adapted to convert the fluid sample into a gas phase to inject the fluid sample into the flowpath as a gas;

a separation column forming part of the flowpath downstream of the controllable expander injector, for separating a plurality of components within the fluid sample; and

a detector located downstream of the separation column, measuring at least one property of the gas, wherein the flowpath, the controllable expander injector, the separation column and the detector are all adapted to operate at ambient temperatures above 75 degrees Celsius, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within a tool housing and adapted to operate at pressures approximate to the incoming downhole pressure of the fluid sample from which the fluid sample was collected.

37. The system according to claim 36, wherein the flowpath, the controllable expander injector, the separation column and the detector are all adapted to operate at ambient temperatures above 100 degrees Celsius.

38. The system according to claim 36, wherein the flowpath, the controllable expander injector, the separation column and the detector are all adapted to operate at ambient temperatures above 150 degrees Celsius.

39. The system according to claim 36, wherein the flowpath, the controllable expander injector, the separation column and the detector are all adapted to operate at pressures above 100 atmospheres.

40. The system according to claim 36, further comprising:

a tool housing constructed and adapted to be deployed in a wellbore in a subterranean rock formation; and

a fluid collection system for obtaining the fluid sample downhole, wherein the flowpath, injector, column and detector are housed within the tool housing and adapted to operate under downhole conditions.

41. The system according to claim 36, further comprising a processing system adapted to calculate from measurements made by the detector a value relating to the amount of at least one component of the fluid sample.

42. A method for chromatographic analysis of a fluid sample at high temperatures, the method comprising the steps of:

converting the fluid sample into a gas phase with a controllable expander injector to inject the fluid sample as a gas into a high pressure flowpath, wherein the flow is adapted to operate at pressures above about 20 atmospheres and operate at ambient temperatures about 100 degrees Celsius;

flowing the injected fluid sample through a separation column;

controlling the temperature of at least the separation column such that the initial temperature of the separation column when the fluid sample enters the separation column is at least 100 degrees Celsius, and the temperature is substantially increase while at least part of the fluid sample remains within the separation column; and

detecting a property of the fluid sample in the flow path with a detector thereby generating measurement data, wherein the flowpath, the controllable expander injector, the separation column and the detector are housed within the tool housing and adapted to operate at pressures approximate to the incoming downhole pressure of the fluid sample from which the fluid sample was collected.

43. The method according to claim 42, wherein the separation column temperature is at least 125 degrees Celsius when the sample enters the separation column.

44. The method according to claim 42, wherein the separation column temperature is at least 150 degrees Celsius when the fluid sample enters separation the column.

45. The method according to claim 42, wherein the flowpath is adapted to operate at pressures above about 100 atmospheres.

46. The method according to claim 42, further comprising the steps of:

containing the fluid sample at high pressure within a container; and

flowing the fluid sample from the container to the controllable expander injector.

47. The method according to claim 42, further comprising collecting the sample from a surface flowline from a wellhead wherein said steps of injecting, flowing and detecting are carried out in close proximity to the wellhead.

48. The method according to claim 42, further comprising the step of collecting the sample downhole wherein said steps of injecting, flowing and detecting are carried out downhole.