Claims
- 1. A process for collecting samples from a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid and a relatively incompressible liquid, comprising the steps of:
controlling the pressure, temperature and velocity of said flow stream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; suppressing formation of aerosols within said separation processes; redirecting said flow stream through a valve system according to a physical starting event into a collection cassette having one or more collection chambers; retaining said liquid phase in said collection chamber and venting said gaseous phase to a waste stream; redirecting said flow stream through said valve system according to a physical stopping event into said waste stream or a second said collection chamber.
- 2. The process according to claim 1, wherein:
said flow stream is the effluent of a supercritical fluid chromatography system or supercritical fluid extraction system.
- 3. The process according to claim 1, further comprising:
transfer tubing carrying said flow stream enhances said separation processes of said monophasic fluid mixture into separate gaseous and liquid phases.
- 4. The process according to claim 3, wherein:
said transfer tubing has inner diameter of approximately 0.030 to 0.063 inches, corresponding to a flowrate in said flow stream of approximately 20 to 100 mL/min.
- 5. The process according to claim 1, wherein:
separation of said incompressible liquid is enhanced by controlling the temperature in said flow stream to suppress aerosols in said collection chamber.
- 6. The process according to claim 1, further comprising: pressure in said flow stream is lowered by the steps of adding restrictors to said flow stream to slow the linear flow rate of said flow stream.
- 7. The process according to claim 1, wherein-further comprising: said physical starting and stopping events result from a detection device in said flow stream.
- 8. The process according to claim 1, wherein: said physical starting and stopping events result from a timing device.
- 9. The process according to claim 1, wherein: said physical starting and stopping events result from a manual signal.
- 10. The process according to claim 1, further comprising:
the volume and direction of said flowstream is controlled with an automatic switching valve system.
- 11. The process according to claim 1, further comprising:
the volume and direction of said flow stream through said flowstream is controlled with a manual switching valve system.
- 12. A process according to claim 1, wherein:
said flowstream collected in said sample collection chamber is pressure controlled to prevent loss of liquid phase due to aerosol formation.
- 13. The process according to claim 1, further comprising:
collecting said liquid phase in a replaceable collection chamber liner housed within said collection chamber, said liner is equilibrated to the pressure inside said collection chamber.
- 14. The process according to claim 1, wherein:
said flow stream discharges from said transfer tube tangentially to the inner wall of said collection chamber.
- 15. The process according to claim 14, further comprising:
a spring wire attached to said transfer tube discharging tangentially to the inner wall of said collection chamber, said spring wire compressing against said inner chamber wall and transferring pressure forces to said transfer tube.
- 16. The process according to claim 1, further comprising:
automatically resetting said collection chamber to an uncontaminated state by robotically replacing a collection liner housed within said collection chamber.
- 17. The process according to claim 1, further comprising:
automatically resetting a plurality of collection chambers integrated as a cassette tray to an uncontaminated state by robotically replacing each cassette tray during sample collection processes.
- 18. The process according to claim 1, further comprising:
removing said liquid phase fluid from said collection chamber through a sample discharge port in said chamber.
- 19. The process according to claim 1, wherein:
said collection system repetitively collects similar fractions from different injected samples into the same chamber.
- 20. A process for collecting samples from a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid and a relatively incompressible liquid, comprising the steps of:
controlling the pressure, temperature, and velocity of said flow stream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; suppressing formation of aerosols within said separation processes; redirecting said flow stream through a valve system according to a physical starting event into a collection cassette having one or more collection chambers; retaining said liquid phase in a replaceable collection liner housed within said collection chamber; equilibrating pressure in said collection chamber with said liner; venting said gaseous phase to a waste stream; redirecting said flow stream through a valve system according to a physical stopping event into said waste stream or a second said collection chamber liner.
- 21. The process according to claim 20, wherein:
said flow stream is the effluent of a supercritical fluid chromatography system or supercritical fluid extraction system.
- 22. The process according to claim 20, further comprising:
transfer tubing carrying said flow stream, said transfer tubing enhancing said separation processes of a monophasic fluid mixture into separate gaseous and liquid phases.
- 23. The process according to claim 20, wherein:
said flow stream flows through transfer tubing having inner diameters of approximately 0.030 to 0.063 inches, corresponding to a flowrate in said flow stream of approximately 20 to 100 mL/min.
- 24. The process according to claim 20, wherein:
collection of said incompressible liquid is enhanced by controlling the temperature in said flow stream to reduce aerosols in said collection chamber.
- 25. The process according to claim 20, further comprising:
pressure in said flow stream is lowered by the steps of adding restrictors to said flow stream to slow the linear flow rate of said flow stream.
- 26. The process according to claim 20, wherein:
said physical starting and stopping events result from a detection device, timing device, or manual signal in said flow stream.
- 27. The process according to claim 20, wherein:
controlling the volume and direction of said flow stream through said valve system with an automatic or a manual switching valve system.
- 28. A process according to claim 20, wherein:
said sample collection chamber is pressure controlled to prevent loss due to turbulence of said liquid phase.
- 29. The process according to claim 20, further comprising:
discharging said flow stream tangentially to the inner wall of said collection chamber through said transfer tubing.
- 30. The process according to claim 20, further comprising:
compressing a spring wire between said transfer tube and the inner wall of said collection chamber, thereby discharging said flow stream tangentially to said inner chamber wall.
- 31. The process according to claim 20, further comprising:
automatically resetting said collection chamber to an uncontaminated state by robotically replacing a collection liner housed within said collection chamber.
- 32. The process according to claim 20, further comprising:
automatically resetting a plurality of collection chambers integrated as a cassette tray to an uncontaminated state by robotically replacing each cassette tray during sample collection processes.
- 33. The process according to claim 20, wherein:
said collection system repetitively collects similar fractions from different injected sample runs into similar said collection chambers.
- 34. A process for collecting samples from a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid and a relatively incompressible liquid, comprising the steps of:
controlling the pressure, temperature and velocity of said flow stream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; suppressing formation of aerosols within said separation processes; directing said flow stream through a valve system according to a physical starting event into a first collection cassette having one or more said collection chambers; retaining said liquid phase in said collection chamber and directing said gaseous phase to a waste stream; automatically resetting said collection chamber to an uncontaminated state; redirecting said flow stream through said valve system according to a physical stopping event into said waste stream or a second uncontaminated collection chamber.
- 35. A process according to claim 34, further comprising:
automatically resetting said cassette to an uncontaminated state by robotically replacing a first collection chamber liner from said cassette with a second uncontaminated collection chamber liner.
- 36. A process according to claim 34, wherein:
automatically resetting said collection chamber to an uncontaminated state comprises the steps: disengaging said lid from said cassette; removing said liner with a robotic arm and placing said liner into a storage area; replacing said liner with said robotic arm with an uncontaminated liner; re-engaging said cassette with said moveable lid.
- 37. A process according to claim 34, wherein:
said lid movement is controlled with a pneumatic actuator.
- 38. An apparatus for collecting samples from a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid and a relatively incompressible liquid, comprising the steps of:
at least one collection chamber having at least one opening; a support frame; a removable lid for said collection chamber having at least one aperture through said lid corresponding to an opening of said collection chamber; at least an inlet and an outlet flow stream path from said collection chamber; said support frame secured to said collection chamber, said lid attached to said support frame and covering said collection chamber opening.
- 39. An apparatus according to claim 38, wherein:
said flow stream paths are transfer tubes comprising an inlet tube carrying said biphase fluid into said collection chamber and an outlet tube carrying a waste stream out of said collection chamber.
- 40. An apparatus according to claim 38, wherein:
said collection chamber is a hollow cylinder secured upright in said support frame, the base of said collection chamber having a sample discharge port, and the top of said chamber having an opening secured in said support frame.
- 41. An apparatus according to claim 38, further comprising:
at least one removable_collection liner housed inside of said collection chamber.
- 42. An apparatus according to claim 38, further comprising:
a plurality of said collection chambers commonly secured within said support frame, thereby forming a cassette bank of said collection containers.
- 43. An apparatus to collect liquid samples from a biphasic flow stream, comprising:
at least one collection chamber with an opening at the top end; a frame; a moveable lid; a plurality of phase transfer points through apertures in said lid corresponding to said open end of said collection chamber; a sample discharge port in said collection chamber; each said collection chamber secured into said frame and said lid covering said collection chamber removably secured to said frame.
- 44. An apparatus according to claim 43, further comprising:
transfer tubes comprising an inlet tube carrying said biphase fluid into said collection chamber and an outlet tube carrying gaseous phase out of said collection chamber.
- 45. An apparatus according to claim 43, further comprising:
at least one removable collection liner housed inside of said collection chamber.
- 46. An apparatus according to claim 43, wherein:
a plurality of said collection chambers commonly secured with said support frame and said lid, thereby forming a cassette bank of said collection containers.
- 47. An apparatus collecting samples from a biphasic flow stream, comprising:
at least one collection chamber open at one end; at least one removable collection liner housed inside of said collection chamber; a support frame; a moveable_lid covering said collection chamber, said lid having apertures through said lid corresponding to the open end of said collection chamber; a sample discharge port through a wall of said collection chamber for removing liquid phase from said chamber; said support frame securing said collection chamber in an upright position.
- 48. An apparatus according to claim 47, wherein:
said collection chamber is cylinder formed from high strength transparent material.
- 49. An apparatus according to claim 47, further comprising:
a plurality of said collection chambers commonly secured with said support frame and said lid, thereby forming a cassette bank of said collection containers.
- 50. An apparatus for collecting samples from a biphasic flow stream, comprising:
means for controlling the pressure, temperature and velocity of a biphasic flowstream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; means for suppressing formation of aerosols within said separation processes; means for redirecting said flow stream through a valve system according to a physical starting event into a collection cassette having one or more collection chambers; means for retaining said liquid phase in said collection chamber and venting waste products to a waste stream; means for redirecting said flow stream through said valve system according to a physical stopping event into said waste stream or a second said collection chamber; means for connecting components of said apparatus.
- 51. The apparatus according to claim 50, wherein:
said flowstream is the effluent of a supercritical fluid chromatography system or supercritical fluid extraction system.
- 52. The apparatus according to claim 50, wherein:
said transfer tubing has inner diameter of approximately 0.040 to approximately 0.063 inches corresponding to flowrate of approximately 20 to 100 mL/min.
- 53. The apparatus according to claim 50, wherein:
one or more heaters control the temperature in said transfer tubing.
- 54. The apparatus according to claim 50, further comprising:
one or more restrictors in said flow stream to slow the linear flow rate of said flow stream.
- 55. The apparatus according to claim 50, wherein:
a detection device in said flow stream controls said physical starting and stopping events.
- 56. The apparatus according to claim 50, further comprising:
a timing device controlling said physical starting and stopping events.
- 57. The apparatus according to claim 50, further comprising:
a manual signal controlling said physical starting and stopping events.
- 58. The apparatus according to claim 50, further comprising:
an automatic switching valve system controlling the volume and direction of said flow stream.
- 59. The apparatus according to claim 50, further comprising:
a manual switching valve system controls the volume and direction of said flow stream.
- 60. The apparatus according to claim 50, further comprising:
a replaceable collection chamber liner housed within said collection chamber, said liner capturing liquid phase inside said collection chamber.
- 61. The apparatus according to claim 50, wherein:
said transfer tubing inside said collection chamber is held tangentially to said collection chamber wall.
- 62. The apparatus according to claim 61, further comprising:
a spring wire attached to said transfer tube held tangentially to said collection chamber wall, said spring wire compressing against a chamber wall and transferring pressure forces to said transfer tube.
- 63. The apparatus according to claim 50, further comprising:
a robotic arm, automatically resetting said collection chambers to an uncontaminated state by replacing collection liners housed within each said collection chamber.
- 64. The apparatus according to claim 50, wherein:
said collection chamber is a hollow cylinder secured upright in said cassette, the top of said chamber having an opening wherein said transfer tubing inserts into said chamber.
- 65. An apparatus collecting samples from a biphasic flow stream, comprising:
a plurality of collection chambers, having at least one opening to each said chamber; a chamber liner for each said chamber; a support frame securing said collection chambers into a cassette bank; at least one actuator connected to said cassette; a moveable lid covering said collection chamber; at least one actuator connected to said moveable lid; said lid having apertures through corresponding to said opening of said collection chambers; a programmable robotic arm; said actuator engages said moveable lid to said frame thereby covering said chambers; said robotic arm exchanges chamber liners within said collection chambers of said cassette.
- 66. An apparatus for collecting samples from a biphasic flow stream, comprising:
means for controlling the pressure, temperature and velocity of said flow stream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; means for suppressing formation of aerosols within said separation processes; means for automatically engaging a lid onto a collection chamber; means for redirecting said flow stream through a valve system according to a physical starting event into a collection cassette having one or more said collection chambers; means for retaining said liquid phase in said collection chamber and venting said gaseous phase to a waste stream; means for automatically disengaging said lid from said collection chamber; means for automatically resetting said collection chamber to an uncontaminated state by robotically replacing said collection chamber within said cassette; means for redirecting said flow stream through said valve system according to a physical stopping event into said waste stream or a second said collection chamber.
- 67. An apparatus according to claim 66, further comprising:
means for automatically moving a cassette away from said lid after said lid has disengaged from said cassette.
- 68. An apparatus according to claim 66, further comprising:
means for automatically resetting replaceable chamber liners housed in at least one said collection chamber to an uncontaminated state by robotically replacing said liners within said collection chamber.
- 69. An apparatus according to claim 66, further comprising:
means for robotically removing a first said liner from said cassette and replaced with a second uncontaminated said chamber liner.
- 70. A process for collecting samples from a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid and a relatively incompressible liquid, comprising the steps of:
controlling the pressure, temperature and velocity of said flow stream to enhance separation processes of a monophasic fluid mixture into separate gaseous and liquid phases; suppressing formation of aerosols within said separation processes; automatically engaging a lid onto wells in a cassette tray; redirecting said flow stream through a valve system according to a physical starting event into wells in a cassette tray; retaining said liquid phase in said wells and venting said gaseous phase to a waste stream; automatically disengaging said lid from said wells; automatically resetting said cassette tray to an uncontaminated state by robotically replacing said cassette tray; redirecting said flow stream through said valve system according to a physical stopping event into said waste stream or a second said cassette tray, collecting a liquid phase sample from said flow stream by robotically moving said lid between said wells in said cassette tray.
- 71. A process according to claim 70, further comprising:
automatically moving a cassette away from said lid after lid has disengaged from said cassette, at which time said collection chamber is robotically removing from said cassette and replaced with a second uncontaminated collection chamber.
- 72. A process according to claim 70, further comprising:
replaceable liners housed in said cassette tray, said liners automatically reset to an uncontaminated state by robotically replacing said liners within said cassette tray.
Parent Case Info
[0001] This application claims the benefit of application Ser. No. 60/154,038, Preparative Supercritical Fluid Chromatography, filed Sep. 16, 1999.
Provisional Applications (1)
|
Number |
Date |
Country |
|
60154038 |
Sep 1999 |
US |
Divisions (1)
|
Number |
Date |
Country |
Parent |
09607316 |
Jun 2000 |
US |
Child |
10066955 |
Feb 2002 |
US |