Thermal isolation system in an analytical instrument

• US 5,663,488 A
• Filed: 05/31/1995
• Issued: 09/02/1997
• Est. Priority Date: 05/31/1995
• Status: Expired due to Fees

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Hewlett-Packard Company (HP Inc.)
• Inventors: Berger, Terry A., Wang, Tak Kui, Baker, James W.
• Primary Examiner(s): Williams, Hezron E.
• Assistant Examiner(s): Politzer, Jay L.
• Application Number:
  US08/456,210
• Time in Patent Office: 825 Days
• Field of Search: 73/23.2, 73/23.21, 73/23.22, 73/23.25, 73/23.26, 73/23.23
• US Class Current: 73/23.25
• CPC Class Codes: B01D 53/228 characterised by specific membranes
• CPC Class Codes: B01D 69/10 Supported membranes; Membrane supports
• CPC Class Codes: B01D 69/108 Inorganic support material
• CPC Class Codes: B01D 71/022 Metals
• CPC Class Codes: B01D 71/02231 Palladium
• CPC Class Codes: C01B 3/505 Membranes containing palladium
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/3007 same temperature for whole column
• CPC Class Codes: G01N 2030/3084 ovens
• CPC Class Codes: G01N 2030/8423 using permeable separator tubes
• CPC Class Codes: G01N 30/30 of temperature

Abstract

Sample analysis in a portable analytical instrument, preferably in the form of a gas chromatograph, benefits from temperature control of one or more thermal zones in the instrument by way of a thermal isolation system that includes a novel pumping assembly to effect a selective amount of thermal isolation of the thermal zone. The pumping assembly includes a pumping element in the form of a tubular or planar palladium structure. The pumping assembly makes use of the unique properties of palladium to allow selective control of a nominal gas pressure within a vacuum cavity. A component system, which may include a separation column and a thermal device for heating and/or cooling the component system, may be provided within the vacuum cavity. The thermal device and the pumping assembly are individually controlled by a control system. The pumping assembly may be operated to allow selective control of the thermal isolation of the thermal zone; alternatively, the component system may be subject to a controlled temperature by operating the thermal device. A sample mixture passing through the separation column may thereby be exposed to a desired temperature profile according to a selected program so that the sample will separate into its components for subsequent detection by a detector.

Claims

1. Apparatus for providing thermal isolation of a component system in an analytical instrument, comprising:

a housing defining a closed cavity and a cavity volume, said closed cavity being subject to pressurization and thereby having a cavity pressure;

means for locating the component system and the housing in a spaced relationship wherein at least a portion of said component system is enclosed within and detached from said housing;

p1 a pumping assembly having a palladium pumping element operatively connected to the cavity for controlling cavity pressure in response to a pressure control signal; and

a controller operatively connected to the pumping assembly for providing said pressure control signal;

wherein said controller includes means for determining a selected cavity pressure and means for providing said pressure control signal in response to said determination so as to control the cavity pressure in the closed cavity, whereby the extent of gas phase heat conduction between said portion of the component system and the housing is selectably controlled.

2. The apparatus of claim 1, further comprising a thermal device operatively connected to the component system and responsive to a thermal control signal for effecting a thermal zone in said portion of the component system.

3. The apparatus of claim 2 wherein the thermal device further comprises a thermoelectric device.

4. The apparatus of claim 2, wherein said pumping assembly further comprises a gas supply system for providing a first flow of hydrogen gas in response to said pressure control signal and a palladium pumping element located with respect to said closed cavity and being responsive to the provision of the first flow for controlling the cavity pressure in the cavity volume.

5. The apparatus of claim 4, wherein the gas supply further comprises means for providing a second flow of gas other than hydrogen, and wherein said first and second flows are provided in response to said pressure control signal for controlling the selectable cavity pressure in the cavity volume.

6. The apparatus of claim 5, wherein the pumping element is provided in the form of a tubular palladium structure.

7. The apparatus of claim 5, wherein the pumping element is provided in the form of a planar palladium structure.

8. The apparatus of claim 4, further comprising:

an active device that is operatively connected to the thermal device;

a temperature sensor for sensing a temperature of the active device and providing a temperature sense signal to said controller;

wherein said controller includes means for determining the current temperature of the active device from the sense signal, comparing the current temperature to a desired temperature, and in response, providing pressure control signal.

9. The apparatus of claim 8, wherein the active device, thermal device, and temperature sensor are integrated in the form of a planar assembly located within the closed cavity.

10. The apparatus of claim 9, wherein the planar assembly further comprises a a gas chromatograph integrated in the planar assembly.

11. The apparatus of claim 9, wherein gas chromatograph is constructed in the form of a planar member and the active device is selected from a group including:

an injection port for receiving a sample and combining the sample with a mobile phase to create a sample mixture;

a separation column having a retentive media therein for effecting separation of a sample chemical mixture into at least one component;

means for providing a selectable flow of a sample mixture in a separation column; and

a detector for detecting the elution of a sample component.

12. An analytical instrument, comprising:

a component system having an active device and a thermal device for altering the temperature of the active device;

a thermal isolation system for receiving the component system and providing temperature control of a thermal zone, said active device being located in the thermal zone, including;

a. a housing defining a closed cavity and a cavity volume, said closed cavity being subject to pressurization and thereby having a cavity pressure, said housing including means for locating the component system and the housing in a spaced relationship wherein at least a portion of said component system is enclosed within and detached from said housing,

b. a gas supply system responsive to a control signal for providing a first flow of hydrogen gas,

c. a pumping assembly having a palladium pumping element located with respect to said closed cavity and operable in response to the provision of first flow for establishing a selectable cavity pressure in the cavity volume and thereby establishing a selected amount of thermal isolation of the thermal zone; and

d. a controller operatively connected to the pumping assembly for providing said pressure control signal;

wherein said controller includes means for determining a selected cavity pressure and means for providing said pressure control signal in response to said determination so as to control the cavity pressure in the closed cavity, whereby the extent of gas phase heat conduction between said portion of the component system and the housing is selectably controlled.

13. The analytical instrument of claim 12, wherein the controller further comprises a memory device for storage and retrieval of a program for effecting a temperature profile.

14. The analytical instrument of claim 12, wherein the controller further comprises an information input device for receiving information representative of a temperature profile.

15. The analytical instrument of claim 12, wherein the controller further comprises a telemetry section for communication of information representative of a temperature profile.

16. The analytical instrument of claim 12, wherein the active device further comprises:

an injection port for receiving a sample and combining the sample with a mobile phase to create a sample mixture;

a separation column having a retentive media therein for effecting separation of the sample mixture into at least one component;

means for providing a selectable flow of the sample mixture in the separation column; and

a detector for detecting the component.

17. A method for providing thermal isolation of a component system in an analytical instrument, comprising the steps of:

providing a control system for supplying at least one of a first and a second control signals;

providing a housing defining a closed cavity and a cavity volume, said closed cavity being constructed to accommodate at least a portion of the component system, the closed cavity being subject to pressurization and thereby having a cavity pressure;

locating the component system and the housing in a spaced relationship wherein the portion of said component system is enclosed within and detached from said housing;

operatively connecting a thermal device to the component system and operating the thermal device in response to the first control signal for effecting a thermal zone in the portion of the component system; and

operatively connecting a pumping assembly having a palladium pumping element to the housing and operating the pumping assembly in response to the second control signal for effecting a selective amount of cavity pressure in the closed cavity, whereby the extent of gas phase heat conduction between the portion of the component system and the housing is selectably controlled.

18. An analytical instrument, comprising:

a component system having an active device and a thermal device for altering the temperature of the active device;

a thermal isolation system for receiving the component system and providing temperature control of a thermal zone, said active device being located in the thermal zone, including;

a. a housing defining a closed cavity and a cavity volume, said closed cavity being subject to pressurization and thereby having a cavity pressure, said housing including means for locating the component system and the housing in a spaced relationship wherein at least a portion of said component system is enclosed within and detached from said housing,

b. a gas supply system responsive to a control signal for providing a first flow of hydrogen gas,

c. a pumping assembly having a palladium pumping element located with respect to said closed cavity and operable in response to the provision of first flow for establishing a selectable cavity pressure in the cavity volume and thereby establishing a selected amount of thermal isolation of the thermal zone;

d. a controller operatively connected to the pumping assembly for providing said pressure control signal;

wherein said controller includes means for determining a selected cavity pressure and means for providing said pressure control signal in response to said determination so as to control the cavity pressure in the closed cavity, whereby the extent of gas phase heat conduction between said portion of the component system and the housing is selectably controlled; and

a telemetry section for communication of information representative of a temperature profile.