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Publication numberUS3213596 A
Publication typeGrant
Publication dateOct 26, 1965
Filing dateMar 5, 1962
Priority dateMar 5, 1962
Publication numberUS 3213596 A, US 3213596A, US-A-3213596, US3213596 A, US3213596A
InventorsGill Harry A
Original AssigneePerkin Elmer Corp
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Chromatography column structure
US 3213596 A
Abstract  available in
Images(4)
Previous page
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Claims  available in
Description  (OCR text may contain errors)

Oct. 26, 1965 H. A. GILL CHROMATOGRAPHY COLUMN STRUCTURE 4 Sheets-Sheet 1 Filed March 5, 1962 HTTOBNEX Oct. 26, 1965 H. A. GILL 3,213,596

CHROMATOGRAPHY COLUMN STRUCTURE Filed March 5, 1962 4 Sheets-Sheet 2 INVENTOR.

Oct. 26, 1965 H. A. GILL 3,213,596

CHROMATOGRAPHY COLUMN STRUCTURE Filed March 5, 1962 4 Sheets-Sheet 3 INVENTOR Harry 1? Gil Oct. 26, 1965 H. A. GILL 3,213,596

CHROMATOGRAPHY COLUMN STRUCTURE v Filed March 5, 1962 4 Sheets-Sheet 4 ZNVENTOR. 97719 H. GJZZ HTTOKNE'X BY W4.

United States Patent 3,213,596 CHROMATOGRAPHY COLUMN STRUCTURE Harry A. Gill, Ridgefield, Conn., assignor to The Perkin- Elmer Corporation, Norwalk, Conn, a corporation of New York Filed Mar. 5, 1962, Ser. No. 177,386 4 Claims. (Cl. 55-208) This invention relates to vapor phase chromatography and, more particularly, to a novel chromatographic column structure.

In chromatography, it is often desirable to program the temperature of the column throughout a range such that components having various boiling points will elute separately from the column. By proper programming, a large number of components may be detected and the usefulness of chromatography is thereby greatly extended. It is also desirable to be able to rapidly cool a column which has undergone such temperature programming. In this manner the column is more readily available for a subsequent analysis.

In prior art chromatography, temperature programming has been attempted by various methods. One such method is to place the column in a heated oven and rely on radiation and convection to provide the necessary heat. The primary ditficulty with this approach is that the thermal coupling between the heat source and the column is very loose. This makes accurate temperature control practically impossible.

Another approach which has been attempted is to wind the column in cylindrical form around a heated mandrel. This approach improves the coupling between the heat source and the column. However, as the column is heated it expands and thereby tends to move away from the mandrel. Thus, much of the improvement in heat coupling is lost and, furthermore, the thermal resistance becomes non-linear.

It is, therefore, the primary object of this invention to provide an improved temperature programmed chromatographic column.

Another object is to provide such a column having improved coupling between such column and the heat source.

Another object is to provide such a' column wherein expansion of the heated column does not destroy the improved coupling.

Another object is to provide such a column which may be rapidly cooled from its maximum temperature to a new starting temperature.

Other objects, features, and advantages will be apparent from the following description taken together with the figures of the attached drawings wherein:

FIG. 1 is a plan view, partially cut away, of an apparatus embodying this invention;

FIG. 2 is an elevational view of the apparatus of FIG.

FIG. 3 is a cross-sectional view of the column assembly taken along line 3-3 of FIG. 1;

FIG. 4 is a plan view, partially cut away, of the heater used with this invention;

FIG. 5 is a cross-section taken along line 5-5 of FIG. 4;

FIG. 6 is a plan view, partially cut away, of a typical column assembly for use with this invention;

FIG. 7 is a View taken along line 77 of FIG. 6;

FIG. 8 is an elevational view showing the mechanical construction of the heater mounting device of this invention; and

FIG. 9 is an overall schematic view of a chromatographic apparatus embodying this invention.

In accordance With this invention, a column is wound so as to lie in a single plane and to allow the two ends of the column to be exposed without crossovers. Such a planar wound column is then mounted in direct contact with a plate-like heater. The column and heater may be maintained in close thermal contact by means of a suitable clamping mechanism. In addition, passages for air or other cooling fluid may be provided along the surfaces of the heater-column combination and suitable means may be provided for passing cooling fluid therethrough.

The manner in which the column structure 11 of this invention is constructed will be best understood by reference to FIGS. 6 and 7. Two thin plates 10, 12 of a suitable heat conducting material such as aluminum are spot welded to opposite sides of a central core assembly made up of segments 14 and 16. The spacing provided between members 10 and 12 is such as to closely contact both sides of the chromatographic column 13 to be employed. Such a column may be either a Golay column or a packed column. The column is wound by passing approximately one-half the tube through the opening between spacers 14 and 16. The twoends of the column are then brought together and are spirally wound about the central core in the manner illustrated. It will be noted that the ends 18, 20 of the column may be brought out from the edge of the assembly without crossing over any previous turns. By this technique substantially the entire length of the column lies in a single plane and in excellent thermal contactwith the thin aluminum discs 10, 12. To complete the assembly, a circumferential spacer 22 is inserted around the edge of the assembly and theentire structure is suitably spot welded or riveted. The particular configuration of this type column will hereinafter be referred to as a double spiral.

The heater employed with this column is constructed as shown in FIG. 4. The heater 24 is a solid aluminum disc. The disc is cast to include a suitable electrical heating element 26 wound in double spiral form as was the column. In addition, a temperature sensing wire 28 is also cast into the assembly between the double spiral turns. Heating element 26 and temperature sensor 28 are insulated electrically from the aluminum disc. Suitable metallic positioning spacers 30 retain the elements in proper alignment during the casting process.

A cross-section of a completed heater assembly is shown in FIG. 3. It will be seen that a base plate 32 is provided with a number of ceramic insulators 34 which are mechanically fastened thereto by wires 35 through the insulators and inserted into holes in plate 32. The function of these spacers is to provide air cooling passages for channeling cool air from inlet air duct 36. The heating element 24 may be hinged as shown in FIG. 8 wherein hinge 38 is of the type that provides a degree of freedom in the vertical direction. Heater 24 may be pivoted downward to the position shown in FIG. 3, where it rests upon the ceramic spacers 34. The completed column assembly llis placed directly upon the surface of heater 24. A cover plate 40 is then positioned over the column. Cover plate 40 carries upon its surface a number of ceramic spacers 42 identical to spacers 34 which similarly form passages for cooling fluid across the surface of column assembly 11. The top and bottom of the complete assembly are covered with rigid heat insulation 44. A clamp mechanism including a U strap 46 and a thumb screw 48 holds the assembly together and provides adequate pressure on the heater-column assembly to insure good thermal contact.

It will be noted that this invention is not restricted to apparatus utilizing a single column. Two columns may advantageously be employed by positioning one above and one below heater 24.

Rapid cooling of the column of this invention is provided by cooling air duct 36 which receives air either from a blower 50 driven by a suitable motor 52 or from a compressed air supply 54. The housing for the heater- 3 column assembly may be of sheet metal provided with additional heat insulation 56 as required in addition to the rigid heat insulation 44.

FIG. 9 illustrates the manner in which the column 13 is connected into a chromatographic system. In this illustration 3. carrier gas supply conduit 58 provides carrier flow to a heated injector block 60. The carrier gas flows' through block 60, past assembly injection point 62 where it picks up the sample to be analyzed. Upon reaching a suitable stream splitter 64 a portion of the carrier-sample combination passes into conduit 66. The remainder is vented through waste line 68. The samplecarrier combination in line 66 passes into inlet 18 of column 13 where separation occurs. Upon leaving column 13 the various components are separately eluted through line 20 and eventually pass to a suitable mixing T 70. Mixing T 70 mixes the elutant with a fuel gas, such as hydrogen, supplied from line 72. The resulting mixture passes to a detector such as flame detector 74. The electrical signal from detector 74 is amplified by amplifier 76 and applied to a suitable recorder 78. Jumper 80, which is in the flow path between column 13 and mixing T 70, is provided in order that a second column may be easily inserted in series with column 13. This is accomplished by merely removing this jumper and connecting the second column inlet and outlet in its place. It will be understood that a detector of any suitable type may be used with this invention. The invention is not limited to use with a flame detector.

By means of this invention, extremely close coupling is provided between the heater and the column. The sensing wire 28 of the heater may be included in a bridge circuit for automatically programming the temperature of the assembly. In this way extremely accurate and linear temperature control is achieved. Furthermore, it

will be apparent that expansion of column 13 does not resultin any decrease in thermal coupling. All expansion of the column takes place in the plane in which it is positioned. The mechanical clamping between the heater and the column also insures against deterioration in thermal coupling. In addition, the provision of aircooling immediately adjacent the column and the heater provides unusually rapid return of the column to a temperature suitable for subsequent sample injection.

It will be apparent that many benefits and advantages accrue from this invention. It will be further apparent that this invention is capable of many variations and modifications without departing from the spirit thereof. It is, therefore, intended that this invention be limited only by the scope of the following claims.

I claim:

1. A chromatographic column assembly comprising:

a support member having a top surface;

a first plurality of spacers on the top surface of said support member defining a first group of air flow channels between said spacers;

a flat heater positioned on said first plurality of spacers;

a cover having a top and bottom side positioned parallel to and above said heater but spaced therefrom;

' a second plurality of spacers on the bottom side of said cover defining a second group of air flow channels between said second plurality of spacers;

and a chromatographic column sub-assembly including .a chromatographic column wound in a double spiral and having substantially its entire length in a common plane and a pair of heat conductive plates, one disposed on each side of said wound column and in direct physical contact with said column, said chromatographic column assembly positioned between said heater and said' second plurality of spacers and in direct physical contact with said heater and said second plurality of spacers.

2. A chromatographic column assembly comprising:

.a support member having a top surface;

a first plurality of spacers on the top surface of said support member defining a first group of air flow channels between said spacers;

a flat heater positioned on said first plurality of spacers;

a cover having a top and bottom side positioned parallel to and above said heater but spaced therefrom;

a second plurality of spacers on the bottom side of said cover defining a second group of air flow channels between said second plurality of spacers;

a chromatographic column sub-assembly including a chromatographic column wound in a double spiral and having substantially its entire length in a common plane and a pair of heat conductive plates, one disposed on each side of said wound column and in direct physical contact with said column, said chromatographic column assembly positioned between said heater and said second plurality of spacers and in direct physical contact with said heater and said second plurality of spacers;

and means for passing a cooling fluid through said first and second groups of air flow channels.

3. A chromatographic column assembly comprising:

a support member having a top surface and a bottom surface;

a first plurality of spacers on the top surface of said support member defining a first group of air flow channels between said spacers;

a flat heater positioned on said first plurality of spacers;

a cover having a top and bottom side positioned parallel to and above said heater but spaced therefrom;

a second plurality of spacers on the bottom side of said cover defining a second group of air flow channels between said second plurality of spacers;

a chromatographic column sub-assembly including a chromatographic column wound in a double spiral and having substantially its entire length in a common plane and a pair of heat conductive plates, one disposed on each side of said wound column and in direct physical contact with said column, said chromatographic column assembly positioned between said heater and said second plurality of spacers and in direct physical contact with said heater and said second plurality of spacers;

a first heat insulator positioned on the bottom surface of said support member;

and a second heat insulator positioned on the top side of said cover.

4. A chromatographic column assembly comprising:

a support member having a top surface and a bottom surface;

a first plurality of spacers on the top surface of said support member defining a first group of air flow channels between the spacers;

a flat heater positioned on said first plurality of spacers;

a cover having a top and bottom side positioned parallel to and above said heater but spaced therefrom;

a second plurality of spacers on the bottom side of said cover defining a second group of air flow channels between said second plurality of spacers;

a chromatographic column sub-assembly including a chromatographic column wound in a double spiral and having substantially its entire length in a common plane and a pair of heat conductive plates, one disposed on each side of said Wound column and in direct physical contact with said column, said chromatographic column assembly positioned between said heater and said second plurality of spacers and in direct physical contact with said heater and said second plurality of spacers;

means for passing a cooling fluid through said first and second group of air flow channels;

a first heat insulator positioned on the bottom surface of said support member;

5 a second heat insulator positioned on the top side of said cover; and a housing surrounding said chromatographic column assembly.

References Cited by the Examiner 5 UNITED STATES PATENTS 480,286 8/92 Serpollett 165-180 X 1,847,573 3/32 Rupp 165-180 X 2,169,852 8/39 Scott. 10 2,281,065 4/42 Lavigne 6217 X 2,300,634 11/42 Schoenfeld. 2,362,163 11/44 Shipman 261146 2,398,818 4/46 Turner 55--67 X 2,469,435 5/49 Hirsch 55-19 X 15 2,833,527 5/58 Kohl et a1. 261- -148 2,841,005 7/58 Coggeshall 55-197 X 2,868,011 1/59 Coggeshall 55-197 FOREIGN PATENTS Canada. Canada. Canada. France.

Great Britain.

OTHER REFERENCES Wisemann et 211.: German application 1,113,319, printed August 31, 1961, KL.421 4/16 (2 pp. dwg. 3 pp. spec.).

REUBEN FRIEDMAN, Primary Examiner.

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US480286 *Nov 20, 1890Aug 9, 1892 Xrateurs
US1847573 *Mar 12, 1930Mar 1, 1932Commercial Iron WorksPlaten for presses with heating coils
US2169852 *Sep 10, 1937Aug 15, 1939Gen ElectricCoffee maker
US2281065 *Dec 17, 1936Apr 28, 1942Lavigne Jean Loumiet EtFluid separation
US2300634 *Apr 26, 1941Nov 3, 1942Comb Eng Co IncTube coils
US2362163 *Dec 20, 1940Nov 7, 1944Raldo E ShipmanCarburetor
US2398818 *Jul 9, 1941Apr 23, 1946Turner Nelson CApparatus for separating gases and the like
US2469435 *Jan 17, 1944May 10, 1949Adler Hirsch AbrahamRegenerable desiccator
US2833527 *Jun 6, 1955May 6, 1958Fluor CorpLiquid and gas contacting columns and their tray structures
US2841005 *Dec 11, 1956Jul 1, 1958Gulf Oil CorpChromatographic method and apparatus
US2868011 *Dec 16, 1955Jan 13, 1959Gulf Research Development CoMultiple-column chromatographic apparatus
US3023835 *Oct 20, 1958Mar 6, 1962Phillips Petroleum CoThermochromatographic analyzer heater
US3035383 *Jan 12, 1959May 22, 1962Phillips Petroleum CoThermochromatographic column
US3043127 *Dec 11, 1958Jul 10, 1962Phillips Petroleum CoThermochromatography heater
US3062037 *Apr 22, 1957Nov 6, 1962Beckman Instruments IncTemperature regulator for chromatographs
US3063286 *Jul 14, 1959Nov 13, 1962Standard Oil CoSample introduction system for gas chromatography apparatus
US3122014 *Jul 5, 1961Feb 25, 1964Murrell R DobbinsChromatography column enclosure
CA478891A *Nov 27, 1951Westinghouse Canada LtdSeparation of gases
CA636078A *Feb 6, 1962Standard Oil CoGas chromatography apparatus
CA636165A *Feb 6, 1962Dow Chemical CoChromatography column
FR553950A * Title not available
GB783713A * Title not available
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US3327520 *Feb 28, 1964Jun 27, 1967Beckman Instruments IncHeated sample injection port
US3363447 *Feb 14, 1966Jan 16, 1968Universal Oil Prod CoMultiple chromatograph column heater unit
US5236668 *Dec 23, 1991Aug 17, 1993Higdon William RDetachable column cartridge gas chromatograph
US5298225 *Jul 30, 1993Mar 29, 1994Microsensor Technology, Inc.Detachable column cartridge gas chromatograph
US5578157 *Sep 28, 1994Nov 26, 1996Microsensor Technology, Inc.Method of fabricating connector
US5601785 *Mar 28, 1994Feb 11, 1997Microsensor Technology, Inc.Connector for detachable column cartridge for gas chromatograph
EP0445967A2 *Feb 28, 1991Sep 11, 1991University Of DaytonImproved gas chromatography methods and apparatus
EP0724722A1 *Dec 23, 1992Aug 7, 1996Technology Inc. MicrosensorDetachable column cartridge for gas chromatograph
WO1993013415A1 *Dec 23, 1992Jul 8, 1993William R HigdonDetachable column cartridge for gas chromatograph
Classifications
U.S. Classification96/106, 73/23.25
International ClassificationG01N30/30, G01N30/00
Cooperative ClassificationG01N30/30, G01N2030/3084
European ClassificationG01N30/30