Claims
- 1. A method for characterizing a polymer sample, the method comprising
withdrawing a polymer sample from a sample container into an injection probe of an auto-sampler, the injection probe being heated to maintain the withdrawn sample at a temperature of not less than about 75° C. while resident in the injection probe, the heated injection probe residing in a first environment maintained at about ambient temperature while withdrawing the polymer sample, loading at least a portion of the withdrawn sample into an injection port or a loading port of a liquid chromatography system, the injection port or loading port being adaptable for fluid communication with a chromatographic column, the chromatographic column residing in a heated second environment maintained at a temperature of not less than about 75° C., injecting the loaded sample into a mobile phase of the liquid chromatography system, maintaining the sample at a temperature of not less than about 75° C. during a period of time including from when the sample is withdrawn from the sample container to when the sample is within the heated second environment, chromatographically separating the injected sample, and detecting a property of the sample or of a component thereof.
- 2. The method of claim 1 further comprising beating the sample container to maintain the polymer sample at a temperature of not less than about 75° C. while the sample is resident in the container.
- 3. The method of claim 1 wherein the injection probe is heated to maintain the withdrawn sample at a temperature of not less than about 100° C. while resident in the injection probe, the heated second environment is maintained at a temperature of not less than about 100° C., and the sample is maintained at a temperature of not less than about 100° C. during a period of time including from when the sample is withdrawn from the sample container to when the sample is injected into the portion of the liquid chromatography system residing in the heated second environment.
- 4. The method of claim 1 wherein the injection probe is heated to maintain the withdrawn sample at a temperature of not less than about 125° C. while resident in the injection probe, the heated second environment is maintained at a temperature of not less than about 125° C., and the sample is maintained at a temperature of not less than about 125° C. during a period of time including from when the sample is withdrawn from the sample container to when the sample is injected into the portion of the liquid chromatography system residing in the heated second environment.
- 5. The method of claim 1 wherein the injection probe is heated to maintain the withdrawn sample at a temperature of not less than about 150° C. while resident in the injection probe, the heated second environment is maintained at a temperature of not less than about 150° C., and the sample is maintained at a temperature of not less than about 150° C. during a period of time including from when the sample is withdrawn from the sample container to when the sample is injected into the portion of the liquid chromatography system residing in the heated second environment.
- 6. The method of claim 1 wherein the injection port or loading port resides in the first environment maintained at about ambient temperature, the method further comprising
advancing the injected sample toward the chromatographic column through a transfer line providing fluid communication between the injection port or loading port and the chromatographic column, and heating the transfer line to maintain the injected sample at a temperature of not less than about 75° C. while resident in the transfer line.
- 7. The method of claim 1 wherein the injection port or the loading port resides in the heated second environment maintained at a temperature of not less than about 75° C.
- 8. A method for characterizing a polymer sample, the method comprising
withdrawing a polymer sample from a sample container into an injection probe of an auto-sampler, the injection probe being heated to maintain the withdrawn sample at a temperature of not less than about 75° C. while resident in the injection probe, the heated injection probe residing in a first environment maintained at about ambient temperature, loading at least a portion of the withdrawn sample into an injection port or a loading port of a flow-injection analysis system, the injection port being adaptable for fluid communication with a continuous-flow detector, injecting the loaded sample into a mobile phase of the flow-injection analysis system, detecting a property of the sample or of a component thereof, and maintaining the sample at a temperature of not less than about 75° C. during a period of time including from when the sample is withdrawn from the sample container to when the property of the sample or of a component thereof is detected.
- 9. A method for characterizing a polymer sample, the method comprising
separating at least one sample component of a polymer sample from other sample components thereof in a chromatographic column residing in a heated environment, maintaining the heated environment at a temperature of not less than about 75° C., allowing at least about ±0.5° C. variation in the temperature of the heated environment, and detecting a property of at least one of the separated sample components with a detector insensitive to the about ±0.5° C. variation in temperature of the heated environment.
- 10. The method of claim 9 wherein the allowed variation in temperature of the heated environment is at least about ±1° C. and the detector is insensitive to the about ±1° C. variation in temperature of the heated environment.
- 11. The method of claim 9 wherein the allowed variation in temperature of the heated environment is at least about ±2° C. and the detector is insensitive to the about ±2° C. variation in temperature of the heated environment.
- 12. The method of claim 9 wherein the allowed variation in temperature of the heated environment is at least about ±5° C. and the detector is insensitive to the about ±5° C. variation in temperature of the heated environment.
- 13. The method of claim 9 wherein the heated environment is maintained to be not less than about 100° C.
- 14. The method of claim 9 wherein the heated environment is maintained to be not less than about 125° C.
- 15. The method of claim 9 wherein the heated environment is maintained to be not less than about 150° C.
- 16. A method for characterizing a polymer sample, the method comprising
preparing a chromatographic column for separation by heating the column from about ambient temperature to about 75° C. in less than about 1 hour, separating at least one sample component of a polymer sample from other sample components thereof in the heated chromatographic column, and detecting a property of at least one of the separated sample components.
- 17. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 75° C. in less than about 30 minutes.
- 18. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 100° C. in less than about 1 hour.
- 19. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 100° C. in less than about 30 minutes.
- 20. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 125° C. in less than about 1 hour.
- 21. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 125° C. in less than about 30 minutes.
- 22. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 150° C. in less than about 1 hour.
- 23. The method of claim 16 wherein the chromatographic column is heated from about ambient temperature to about 150° C. in less than about 30 minutes.
- 24. A method for characterizing a polymer sample, the method comprising
loading a polymer sample into a liquid chromatography system, maintaining the loaded polymer sample at a temperature of not less than 75° C., eluting one or more sample components of the polymer sample with a mobile-phase eluant having a temperature of not less than about 75° C., controlling the composition of the mobile-phase eluant to vary over time to separate at least one sample component of the sample from other sample components thereof, and detecting a property of at least one of the separated sample components.
- 25. The method of claim 24 wherein the loaded polymer sample is maintained at a temperature of not less than 100° C. and the mobile-phase eluant has a temperature of not less than about 100° C.
- 26. The method of claim 24 wherein the loaded polymer sample is maintained at a temperature of not less than 125° C. and the mobile-phase eluant has a temperature of not less than about 125° C.
- 27. The method of claim 24 wherein the loaded polymer sample is maintained at a temperature of not less than 150° C. and the mobile-phase eluant has a temperature of not less than about 150° C.
- 28. A method for characterizing a polymer sample, the method comprising
loading a polymer sample into a liquid chromatography system, eluting one or more sample components of the polymer sample with a mobile-phase eluant, controlling the temperature of the mobile-phase eluant to vary over time to separate at least one sample component of the sample from other sample components thereof, and detecting a property of at least one of the separated sample components.
- 29. The method of claim 28 wherein the loaded polymer sample comprises at least one precipitated sample component.
- 30. The method of claim 28 wherein the polymer sample comprises one or more sample components that are insoluble at a temperature of less than about 75° C.
- 31. The method of claim 28 wherein the polymer sample comprises one or more sample components that are insoluble at a temperature of less than about 100° C.
- 32. The method of claim 28 wherein the polymer sample comprises one or more sample components that are insoluble at a temperature of less than about 125° C.
- 33. The method of claim 28 wherein the polymer sample comprises one or more sample components that are insoluble at a temperature of less than about 150° C.
- 34. The method of claim 28 wherein the chromatographic column comprises a stationary phase and the polymer sample comprises one or more sample components that are non-desorbing from the stationary phase at a temperature of less than about 75° C.
- 35. The method of claim 28 wherein the chromatographic column comprises a stationary phase and the polymer sample comprises one or more sample components that are non-desorbing from the stationary phase at a temperature of less than about 100° C.
- 36. The method of claim 28 wherein the chromatographic column comprises a stationary phase and the polymer sample comprises one or more sample components that are non-desorbing from the stationary phase at a temperature of less than about 125° C.
- 37. The method of claim 28 wherein the chromatographic column comprises a stationary phase and the polymer sample comprises one or more sample components that are non-desorbing from the stationary phase at a temperature of less than about 150° C.
- 38. The method of claim 28 further comprising controlling the temperature of the chromatographic column.
- 39. A method for characterizing a polymer sample, the method comprising
loading a polymer sample into a liquid chromatography system having a chromatographic column, eluting the column with a mobile phase, controlling the temperature of the column while eluting the column with the mobile phase such that at least one sample component of the loaded sample is separated from other sample components thereof, and detecting a property of at least one of the separated sample components.
- 40. The method of claim 39 wherein the mobile phase is supplied to the column at about a constant temperature.
- 41. The method of claim 39 further comprising controlling the temperature of the column while loading the sample onto the column.
- 42. The method of claim 39 further comprising controlling the temperature of the column while loading the sample such that at least one sample component precipitates or adsorbs onto the stationary phase.
- 43. An apparatus for automated sampling of polymer samples for characterization, the apparatus comprising
a probe having a surface defining a sample-cavity and an inlet port for fluid communication between the sample cavity and a polymer sample, the probe being adapted for fluid communication with an injection port or a loading port of a continuous-flow polymer characterization system, a microprocessor for controlling three-dimensional motion of the probe between various spatial addresses, a pump for withdrawing a polymer sample into the probe, and a temperature-control element in thermal communication with the probe for maintaining a polymer sample residing in the probe at a predetermined temperature or within a predetermined range of temperatures.
- 44. The apparatus of claim 43 wherein the temperature-control element is a heating element for maintaining a sample residing in the probe at a temperature of not less than about 75° C.
- 45. The apparatus of claim 43 wherein the temperature-control element is a heating element for maintaining a sample residing in the probe at a temperature of not less than about 100° C.
- 46. The apparatus of claim 43 wherein the temperature-control element is a heating element for maintaining a sample residing in the probe at a temperature of not less than about 125° C.
- 47. The apparatus of claim 43 wherein the temperature-control element is a heating element for maintaining a sample residing in the probe at a temperature of not less than about 150° C.
- 48. The apparatus of claim 43 wherein the temperature-control element is a cooling element.
- 49. A liquid chromatography system for characterizing a polymer sample, the system comprising
an enclosure defining a heated environment, the heated environment being maintained at a temperature of not less than about 75° C. and having at least about ±0.5° C. variation in temperature, a chromatographic column residing in the heated environment, the chromatographic column comprising a surface defining a pressurizable separation cavity, an inlet port for receiving a mobile phase and for supplying a polymer sample to the separation cavity, an effluent port for discharging the mobile phase and the polymer sample or separated components thereof from the separation cavity, and a stationary-phase within the separation cavity, an injection port or a loading port adaptable for fluid communication with the chromatographic column for injecting polymer samples into the mobile phase, a reservoir in fluid communication with the inlet port of the chromatographic column for providing a mobile phase thereto and adaptable for fluid communication with the injection port, and a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, the detector being insensitive to variations in temperature of about ±0.5° C.
- 50. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 100° C.
- 51. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 125° C.
- 52. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 150° C.
- 53. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 100° C. and has at least about ±1° C. variation in temperature, the detector being insensitive to the variations in temperature of about ±1° C.
- 54. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 100° C. and has at least about ±2° C. variation in temperature, the detector being insensitive to the variations in temperature of about ±2° C.
- 55. The system of claim 49 wherein the heated environment is maintained at a temperature of not less than about 100° C. and has at least about ±5° C. variation in temperature, the detector being insensitive to the variations in temperature of about ±5° C.
- 56. The system of claim 49 wherein the detector is an evaporative light scattering detector.
- 57. A liquid chromatography system for characterizing a po lym er sample, the system comprising
an enclosure defining a heated environment, the heated environment being maintained at a temperature of not less than about 75° C., a chromatographic column residing in the heated environment, the chromatographic column comprising a surface defining a pressurizable separation cavity, an inlet port for receiving a mobile phase and for supplying a polymer sample to the separation cavity, an effluent port for discharging the mobile phase and the polymer sample or separated components thereof from the separation cavity, and a stationary-phase within the separation cavity, an injection port adaptable for fluid communication with the chromatographic column for injecting polymer samples into the mobile phase, a first reservoir for containing a first mobile phase fluid, a second reservoir for containing a second mobile phase fluid, a mixing zone adaptable for fluid communication with the first reservoir and the second reservoir for mixing of the first and second mobile phases to form a mobile-phase eluant having compositions or temperatures that can vary over time, the mixing zone being further adaptable for fluid communication with the inlet port of the chromatographic column for eluting one or more sample components of the sample with the mobile-phase eluant to separate at least one sample component of the sample from other sample components thereof, and a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components.
- 58. The system of claim 57 further comprising a third reservoir for containing a third mobile-phase fluid, the third reservoir being adaptable for fluid communication with the mixing zone for mixing of the third mobile-phase fluid with one or both of the first or second mobile-phase fluids.
- 59. The system of claim 57 wherein the mixing zone is directly upstream of the column inlet port.
- 60. The system of claim 57 wherein the column comprises two inlet ports and the mixing zone is within the column.
- 61. A liquid chromatography system for characterizing a polymer sample, the system comprising
a chromatographic column comprising a surface defining a pressurizable separation cavity, an inlet port for receiving a mobile phase and for supplying a polymer sample to the separation cavity, an effluent port for discharging the mobile phase and the polymer sample or separated components thereof from the separation cavity, and a stationary phase within the separation cavity, an injection port or a loading port adaptable for fluid communication with the chromatographic column for injecting polymer samples into the mobile-phase, a reservoir for containing a mobile phase fluid, the reservoir being adaptable for fluid communication with the inlet port of the chromatographic column, a heater for controlling the temperature of the mobile-phase fluid or for controlling the temperature of the column, such that one or more sample components of the polymer sample can be eluted with a mobile-phase fluid having a temperature that varies over time to separate at least one sample component of the sample from other sample components thereof, and a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components.
- 62. The system of claim 61 further comprising
an enclosure defining a heated environment in which the chromatographic column resides, the heated environment being maintained at a temperature of not less than about 75° C.,
- 63. The system of claim 62 wherein the heated environment is maintained at a temperature of not less than about 100° C.
- 64. The system of claim 62 wherein the heated environment is maintained at a temperature of not less than about 125° C.
- 65. The system of claim 62 wherein the heated environment is maintained at a temperature of not less than about 150° C.
- 66. The system of claim 61 wherein the heater is a heating element in thermal communication with the reservoir.
- 67. The system of claim 61 wherein the heater is a heating element in thermal communication with a mobile-phase fluid transfer line.
- 68. The system of claim 61 wherein the heater is an enclosure defining a heated environment in which a length of a mobile-phase fluid transfer line resides.
- 69. The system of claim 61 wherein the heater is a heating element in thermal communication with the chromatographic column.
Parent Case Info
[0001] This application claims priority under 35 U.S.C. Sec. 119(e) to U.S. Provisional Application Ser. No. 60/080,652, filed Apr. 3, 1998 by Safir et al., which is hereby incorporated by reference for all purposes.
Provisional Applications (1)
|
Number |
Date |
Country |
|
60080652 |
Apr 1998 |
US |
Divisions (1)
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Number |
Date |
Country |
Parent |
09285333 |
Apr 1999 |
US |
Child |
09866428 |
May 2001 |
US |