HIGH PRESSURE AND HIGH TEMPERATURE CHROMATOGRAPHY

• US 20090151426A1
• Filed: 12/17/2007
• Published: 06/18/2009
• Est. Priority Date: 12/17/2007
• Status: Active Grant

• Current Assignee: Schlumberger Technology Corporation (SLB)
• Original Assignee: Schlumberger Technology Corporation (SLB)
• Inventors: Raghuraman, Bhavani, Paso, Kristofer Gunnar, Shah, Jagdish, Bostrom, Neil William, Zhdaneev, Oleg
• Granted Patent: US 8,028,562 B2
• Time in Patent Office: Days
• US Class Current: 73/23.350
• 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 sample comprising:

a flowpath adapted to flow a mobile gas phase and the sample at high pressures;

an injector adapted to inject the sample into the flowpath as a gas;

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

a detector located downstream of the column, measuring at least one property of the gas, thereby generating measurement data representing properties of at least one component of the fluid sample; 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. A system according to claim 1, wherein the system is adapted to operate at pressures above about 20 atmospheres.

3. A system according to claim 2, wherein the system is adapted to operate at pressures above about 100 atmospheres.

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

5. A system according to claim 1, 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.

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

7. A system according to claim 6, wherein the system is in close proximity to the wellhead.

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

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

11. A 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 a component, volume concentration of a component, and ratio of components.

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

injecting the sample as a gas into a high pressure flowpath;

flowing the injected sample through a separation column;

detecting a property of the 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 sample.

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

14. A method according to claim 13, wherein the flowpath is adapted to operate at pressures above about 100 atmospheres.

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

16. A 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. A method according to claim 12, 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.

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

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

containing the sample at high pressure within a container; and

flowing the sample from the container to the injector.

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

21. A 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 a component, volume concentration of a component, and ratio of components.

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

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

an injector adapted to inject the fluid sample into a flowpath;

a separation column adapted to operate at pressures above about 20 atmospheres, forming part of the flowpath downstream of the 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 column, the detector adapted to measure properties of the fluid sample.

23. A 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. A 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 a component, volume concentration of a component, and ratio of components.

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

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

27. A 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. A system according to claim 22, further comprising a tap in fluid communication with a surface flowline carrying produced fluids and said injector.

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

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

a fluid collection system for obtaining a fluid sample downhole;

an injector housed within the housing adapted to inject the downhole fluid sample into a flowpath;

a separation column forming part of the flowpath downstream of the injector, housed within the housing adapted to separate a plurality of components within the downhole fluid sample; and

a detector housed within the column located downstream of the column, the detector adapted to measure properties of the downhole fluid sample.

30. A 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. A 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 fluid sample.

32. A 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 a component, volume concentration of a component, and ratio of components.

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

35. A 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 sample at high ambient temperatures comprising:

a flowpath adapted to flow a mobile gas phase and the sample;

an injector adapted to inject the sample into the flowpath;

a separation column forming part of the flowpath downstream of the injector, for separating a plurality of components with the sample; and

a detector located downstream of the column, measuring at least one property of the gas, wherein the flowpath, the injector, the separation column and the detector are all adapted to operate at ambient temperatures above 75 degrees Celsius.

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

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

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

40. A 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. A system according to claim 36, 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.

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

injecting the sample as a gas into a high pressure flowpath;

flowing the injected sample through a separation column;

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

detecting a property of the sample in the flow path with a detector thereby generating measurement data.

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

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

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

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

containing the sample at high pressure within a container; and

flowing the sample from the container to the injector.

47. A 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. A 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.