Temperature controlling apparatus for use with pore volume and surface area analyzers

Abstract

An apparatus for maintaining a constant temperature within a vessel immersed in a liquid by surrounding a portion of the vessel, extending above the surface of the liquid, with a wick. The wick conducts liquid up to a predetermined point on the vessel and maintains the liquid at that point, regardless of changes in the level of the liquid due to evaporation. The wick is encased within a layer of heat insulating or heat conducting material to further aid in maintaining a constant temperature within the vessel. A second embodiment, including alternating layers of heat conducting and heat insulating material, is disclosed for increased temperature control. The disclosed apparatus is particularly useful for maintaining a constant temperature within a vessel attached to a scientific instrument, such as a port volume and surface area analyzer.

We claim: 
     
       1. A method of cooling a sample contained in a vessel, comprising the steps of: immersing said vessel in a container of volatile cooling liquid with a portion of said vessel extending above the surface of said liquid; and   conducting said liquid .Iadd.through a wick .Iaddend.from a location at or below the surface of said liquid in said container along said vessel to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid, .Iadd.said wick maintaining a lower than ambient temperature at the surface of said vessel along the entire length of said wick.Iaddend..   
     
     
       2. The method of claim 1 wherein said step of conducting said liquid along said vessel comprises conducting said liquid by capillary action. 
     
     
       3. The method of claim 2, further comprising the step of thermally shielding said liquid being conducted along said vessel from ambient temperature .Iadd.with an insulating layer contacting the outer surface of said wick.Iaddend.. 
     
     
       4. The method of claim 3, wherein said step of shielding said liquid from ambient temperature comprises conducting ambient heat to the surface of said liquid in said container. 
     
     
       5. An apparatus for cooling a sample contained in an elongate vessel, comprising: a container of volatile cooling liquid, said vessel being immersed in said liquid and extending above the surface of said liquid; and   .[.means.]. .Iadd.a wick connected to said vessel .Iaddend.for conducting said liquid from a location at or below the surface of said liquid in said container along said vessel to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid.Iadd., said wick maintaining a lower than ambient temperature at the surface of said vessel along the entire length of said wick.Iaddend..   
     
     
       6. The apparatus of claim 5, wherein said .[.means for conducting said liquid.]. .Iadd.wick .Iaddend.comprises means for conducting said liquid by capillary action. 
     
     
       7. The apparatus of claim 6, wherein said means for conducting said liquid by capillary action comprises .[.a wick including.]. connected capillary passageways .[.and.]. .Iadd.in said wick, said wick .Iaddend.extending from below the surface of said liquid to said predetermined point. 
     
     
       8. The apparatus of claim 7, wherein said capillary passageways have an average diameter of about 20 microns. 
     
     
       9. The apparatus of claim 7, further comprises a thermally insulating layer contacting the outer surface of said wick and extending below the surface of said liquid. 
     
     
       10. The apparatus of claim 7, wherein said wick comprises a sleeve surrounding said vessel, and further comprising: an insulating sleeve surrounding the outer surface of said wick; and   a heat conducting sleeve surrounding said first insulating sleeve.   
     
     
       11. The apparatus of claim 10, wherein said insulating sleeve comprises epoxy-filled woven glass filaments. 
     
     
       12. The apparatus of claim 11, wherein said heat conducting sleeve comprises a heat conductive metal. 
     
     
       13. The apparatus of claim 12, wherein said metal comprises copper. 
     
     
       14. The apparatus of claim 7, wherein said wick comprises fibrous material. 
     
     
       15. The apparatus of claim 14, wherein said wick comprises refractory fibers. 
     
     
       16. The apparatus of claim 14, wherein said wick comprises spun kaolin clay. 
     
     
       17. The apparatus of claim 14, wherein said wick comprises glass fibers. 
     
     
       18. The apparatus of claim 14, wherein said wick comprises cellulose fibers. 
     
     
       19. The apparatus of claim 7, wherein said wick comprises packed particles. 
     
     
       20. The apparatus of claim 7, wherein said wick comprises porous ceramic material. 
     
     
       21. The apparatus of claim 7, wherein said liquid comprises liquid nitrogen. 
     
     
       22. The apparatus of claim 7, wherein said wick comprises a material capable of retaining capillary properties upon being cooled to the temperature of liquid nitrogen. 
     
     
       23. The apparatus of claim 7, wherein said wick comprises a sleeve surrounding said vessel, and further comprises an outer sleeve of material impervious to said liquid, surrounding said wick. 
     
     
       24. The apparatus of claim 23, wherein said outer sleeve comprises a heat insulating material. 
     
     
       25. The apparatus of claim 24, wherein said outer sleeve comprises epoxy-filled woven glass filaments. 
     
     
       26. The apparatus of claim 24, wherein said outer sleeve comprises a refractory material. 
     
     
       27. The apparatus of claim 24, wherein said wick and sleeve are one with the inner region being porous and the outer surface fused into an impermeable barrier. 
     
     
       28. The apparatus of claim 23, wherein said outer sleeve comprises a heat conducting material. 
     
     
       29. The apparatus of claim 23, wherein said outer sleeve comprises an impervious layer formed of the material of said wick. 
     
     
       30. The apparatus of claim 5, wherein said predetermined point is as much as 10 inches above the surface of said liquid. 
     
     
       31. The apparatus of claim 5, wherein said said liquid comprises liquid nitrogen. 
     
     
       32. An apparatus for cooling a sample contained in an elongate vessel comprising: a container of a volatile cooling liquid, said vessel being immersed in said liquid and extending above the surface of said liquid; and   .[.conducting means.]. .Iadd.a wick connected to said vessel .Iaddend.for conducting said liquid from a location at or below the surface of said liquid in said container to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid, said .[.conducting means.]. .Iadd.wick .Iaddend.extending, during conduction of said liquid from a location at or below the surface of said liquid to said point.Iadd., said wick maintaining a lower than ambient temperature at the surface of said vessel along the entire length of said wick.Iaddend..   
     
     
       33. A method of cooling a sample contained in a vessel, comprising the steps of: immersing said vessel in a container of a volatile cooling liquid with a portion of said vessel extending above the surface of liquid; and   conducting said liquid .Iadd.through a wick .Iaddend.from a location at or below the surface of said liquid in said container along said vessel to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid, while said container contains at least a predetermined minimum amount of said liquid.Iadd., said wick maintaining a lower than ambient temperature at the surface of said vessel along the entire length of said wick.Iaddend.. .Iadd.34. An apparatus for cooling a sample contained in a vessel, comprising:   a container of volatile cooling liquid, said vessel being immersed in said liquid and extending above the surface of said liquid;   liquid conducting means for conducting said liquid from a location at or below the surface of said liquid in said container along said vessel to a predetermined point on said vessel above the surface of said liquid, regardless of changes in the level of the surface of said liquid; and   heat conducting means for conducting ambient heat to the surface of said liquid in said container to thermally shield said liquid conducting means   
     
     
        from ambient temperature. .Iaddend. .Iadd.35.  An apparatus for cooling a sample contained in a vessel, comprising: a container of volatile cooling liquid, said vessel being immersed in said liquid and extending above the surface of said liquid;   a layer of wick material for conducting said liquid from a location at or below the surface of said liquid in said container along said vessel to a predetermined point on said vessel above the surface of said liquid regardless of changes in the level of the surface of said liquid; and   a liquid impermeable layer contacting the outer surface of said wick material, said liquid impermeable layer being open to said liquid at or below the surface of said liquid and open to the ambient atmosphere at   
     
     
        said point on said vessel. .Iaddend. .Iadd.36.  An apparatus for cooling a sample contained in a vessel, comprising: a container of volatile cooling liquid, said vessel being, immersed in said liquid and extending above the surface of said liquid; and   a wick conforming in shape to at least a portion of said vessel, said wick being attached to said vessel so as to extend from a location at or below the surface of said liquid in said container along said vessel to a predetermined point on said vessel above the surface of said liquid;   said wick conducting said liquid from a location at or below the surface of said liquid in said container to said predetermined point, regardless of   
     
     
        changes in the level of the surface of said liquid. .Iaddend. .Iadd.37. The apparatus of claim 36, wherein said wick is removably attached to said 
     
     
        vessel. .Iaddend. .Iadd.38.  An apparatus for cooling a sample contained in a vessel, comprising: a container of volatile cooling liquid, said vessel defining a tubular portion immersed in said liquid and extending above the surface of said liquid; and   a sleeve of wick material inserted onto said tubular portion of said vessel so as to extend from a location at or below the surface of said liquid in said container along said vessel to a predetermined point on said vessel above the surface of said liquid;   said wick material conducting said liquid from a location at or below the surface of said liquid in said container to said predetermined point, regardless of changes in the level of the surface of said liquid.   
     
     
        .Iaddend. .Iadd.39.  The apparatus of claim 38, wherein said wick is 
     
     
        removably attached to said vessel. .Iaddend. .Iadd.40.  An apparatus for cooling a sample contained in a vessel positioned in a container of volatile cooling liquid of the type in which the vessel is immersed partly in said cooling liquid and cooling liquid is conducted to non-immersed parts of the vessel, comprising: a wick connected to said vessel and extending from under the surface of said cooling liquid to above the surface, said wick maintaining a lower than ambient temperature at the surface of said vessel along the entire length of said wick. .Iaddend. .Iadd.41. A method of cooling a sample, comprising the steps of:   placing said sample in a vessel, said vessel defining an elongate tubular portion thereof;   inserting a sleeve of wick material over said tubular portion of said vessel until said sleeve extends from a predetermined point along said tubular portion downwardly along said tubular portion;   immersing said vessel into a container of a volatile cooling liquid until said sleeve of wick material is partially immersed in said cooling liquid and said predetermined point is above the surface of said cooling liquid;   conducting said liquid through said wick from a location at or below the surface of said liquid in said container to said predetermined point; and   maintaining the position of said vessel with respect to said container regardless of changes in the level of the surface of said cooling liquid.   
     
     
        .Iaddend. .Iadd.42.  A method of cooling a sample contained in a vessel, comprising the steps of: immersing said vessel in a container of volatile cooling liquid with a portion of said vessel extending above the surface of said liquid;   conducting said liquid by capillary action from a location at or below the surface of said liquid in said container along said vessel to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid; and   thermally shielding said liquid being conducted along said vessel from ambient temperature by conducting ambient heat to the surface of said liquid in said container. .Iaddend. .Iadd.43. An apparatus for cooling a sample contained in an elongate vessel, comprising:   a container of volatile cooling liquid, said vessel being immersed in said liquid and extending above the surface of said liquid; and   means for conducting said liquid by capillary action from a location at or below the surface of said liquid in said container along said vessel to a predetermined point along the length of said vessel, said point being above the surface of said liquid, regardless of changes in the level of the surface of said liquid, comprising a wick including connected capillary passageways and extending from below the surface of said liquid to said predetermined point. .Iaddend. .Iadd.44. The apparatus of claim 43, further comprising a thermally insulating layer contacting the outer surface of said wick and extending below the surface of said liquid. .Iaddend. .Iadd.45. The apparatus of claim 43, wherein said wick comprises a sleeve surrounding said vessel, and further comprises an outer sleeve of material impervious to said liquid, surrounding said wick. .Iaddend. .Iadd.46. The apparatus of claim 45, wherein said outer sleeve comprises a   
     
     
        heat conducting material. .Iaddend. .Iadd.47.  The apparatus of claim 45, wherein said outer sleeve comprises an impervious layer formed of the material of said wick. .Iaddend.