US3363447A

US3363447A - Multiple chromatograph column heater unit

Info

Publication number: US3363447A
Application number: US526979A
Authority: US
Inventors: Richard K Severs
Original assignee: Universal Oil Products Co
Current assignee: Universal Oil Products Co
Priority date: 1966-02-14
Filing date: 1966-02-14
Publication date: 1968-01-16
Anticipated expiration: 1985-01-16

Description

Jan. 16; 1968 R. K. SEVERS MULTIPLE CHROMATOGRAPH COLUMN HEATER UNIT Filed Feb. 14, 1966 Figure 'IIIIIIIIIIIIIIIJ United States Patent Ofilice 3,363,447 Patented Jan. 16, 1968 3,363,447 MULTIPLE CHROMATOGRAPH COLUMN HEATER UNIT Richard K. Severs, Mount Prospect, Ill., assignor to Universal Bil Products Company, Des Plaines, 111., a corporation of Delaware Filed Feb. 14, 1966, Ser. No. 526,979 7 Claims. (Cl. 7323.1)

The present invention is directed to a multiple column heater unit and more particularly to the design and construction of a heating unit which provides for the rapid substitution of one gas chromatograph column for another in the oven section of the unit.

chromatograph columns, as used in a gas-liquid chromatography, liquid-liquid chromatography, and gas-solid chromatography, contain a suitable solid absorbent material in granular form to effect a separation of a fluid stream or, alternatively, they utilize a thin liquid film held over the exposed surface of an inert support material. In either case, the fluid sample being analyzed is introduced into the column in a suitable carrier fluid so that there is a selective adsorption or liquid partitioning to provide separations analogous to distillation. Also, in either type of separation, the continuous flow of the fluid stream provides for the sequential removal of components from the column and their passage to suitable detector means which can sense the relative volatilities, molecular weights, or other properties of such components.

In most analytical laboratories it is generally necessary to have several chromatograph units in order to accommodate various types of analyses which must be run through different types of sizes of columns; however, in many instances it would be possible to use the same heater or oven section if it were possible to effect a rapid change over of chromatograph columns and not have to wait for a cooling down of the entire heater unit. In other words, with a rapid substitution of one column for another in an already hot oven section, there can be carried out successive analysis operations without necessarily utilizing an entirely separate heating unit or chromatograph unit.

Thus, it may be considered a principal object of the present invention to provide a multiple column heating unit which is constructed and arranged to provide for the rapid substitution of one column for another.

It is a further object of the present invention to provide a heater unit having accompanying movable column support means or end manifold means for holding a plurality of columns, where such support means is movable with respect to the oven section of the unit and, in addition, movable Wall sections are provided for the oven unit whereby there may be a rapid substitution of one column for another into the interior thereof.

Broadly, the present invention may be considered to provide a multiple column heating unit which provides for the selective insertion of one chromatograph column of a plurality thereof into the oven portion of the unit and comprises in combination, an elongated oven cham ber having a heat supply source for heating the interior thereof, elongated movable Wall portions for such chamher, a plurality of spaced apart separate columns supported by and extending from movable end mounting means, with the latter being positioned in combination with said heating chamber to translate with respect thereto and in turn permit any one of said plurality of columns to be positioned interiorly within said oven chamber upon temporarily moving aside said wall portions of said chamber, and attachment means at the ends of each of said plurality of columns for the connection thereof to a gas supply line.

Generally, the heating chambers or oven sections utilized in connection with chromatograph analyzing equipment are of the electrical resistance heater type of construction whereby there may be a close control of the heat output by suitable electrical control means. Also, present constructions generally provide for the placement of an open heater unit over a mounted chromatograph column or the insertion of one or more coiled columns through the top of an oven chamber. In contrast, the multiple column heater unit, as provided by the present invention, is normally arranged to be in a fixed position, normally as a horizontally arranged heating chamber having combined therewith a movable column supporting means such that the transverse movement of the latter will permit the simultaneous removal of one column and the insertion of another into the heating zone. In order to provide for the substitution of columns it is of course necessary that one or more wall sections of the heating chamber be movable for the temporary opening of such chamber portion while the substitution of columns takes place. For example, opposing wall sections of an elongated oven section may be hingedly attached to a remaining fixed portion of the oven unit whereby there may be a temporary lifting of such hinged sections while the translating movement of the column support means takes place to substitute one column for another within the central portion of the oven section.

Various types of movable support members may be utilized, as well as various types of movements provided, so as to effect the removal and insertion of column sections. For instance, in one type of unit, there may be a plurality of columns supported from at least one rotating disc-like support member such that the rotation of the latter around a central axis will effect the movement of one column out of the oven section and the introduction of another into it, as long as the column sections are located at equal radial distances fromthe axis of rotation and at suitable spaced distances from one another to permit a final positioning of the new column within the central portion of the oven. In another instance, the plurality of chromatograph columns may be mounted to project between or perpendicularly outwardly from at least elongated support means which in turn is movably mounted with respect to the oven section so as to have translative movement across the end of the oven section and thus provide for the removal of one column and the substitution of another from one unidirectional movement. Inasmuch as various sizes, lengths and configurations of packed columns are used in chromatograph analysis operations, it is not intended that the plurality of columns mounted on the support means for any one improved multiple column unit will be of the same size and type. In other words, each multiple column unit may have several sizes and types of packed column sections whereby the proper translative movement of the support means, following the opening of the movable wall sections of the oven chamber, will permit the selective removal of one column and the substitution of a different desired type into a still hot oven section.

Reference to the accompanying diagrammatic drawing and the following description thereof will serve to illustrate a broad concept of the present invention as well as point out additional advantageous features in connection therewith.

FIGURE 1 of the drawing is a sectional elevational view of one embodiment of a multiple column heating unit providing for the mounting of a plurality of separate chromatograph columns between rotatable end support members.

FIGURE 2 of the drawing is also a sectional elevational view, as indicated by the line 2-4 in FIGURE 1, indicating how the rotational translative movement of the columns with respect to the oven portion of the unit permits the substitution of one column for another.

FIGURE 3 of the drawing indicates in a partial sectional view how a plurality of columns may be mounted from a single rotative disc-like support member, with the column sections fabricated to have their respective end portions terminate at the same end of the oven section and exteriorly of a single common support member.

FIGURE 4 of the drawing indicates diagrammatically still another modified form of a multiple column heating unit, where the various column sections being mounted perpendicularly from an elongated rectangular column support means in turn designed and supported to move horizontally with respect to the oven section.

Referring now particularly to FIGURES 1 and 2 of the drawing, there is shown a multiple column heating unit having a heating chamber or oven section 1 supported by means of brackets 2 which in turn extend upwardly from a suitable supporting base or stand 3. As best shown by FIGURE 2, the oven chamber 1 has elongated wall portions 1 which are hingedly connected to the fixed shell portion of oven 1 by hinges 4 so that by temporarily raising such side portions 1 there can be a rapid substitution of a diiferent chromatograph column, into the heating zone. Each of the oven sections may be provided with suitable electrical resistance coil heating (not shown) which in turn is supplied with electrical energy through supply lines indicated as 5. The electrical heating may of course be controlled by suitable monitoring or programming means that is apart of a complete chromatograph unit, so that it is not intended to limit the present invention to any particular type of electrical heating or control system.

A central axle 6 is shown extending between bearing means 7 in the ends of the stand 3 whereby there is an axial supporting means for rotatable column supporting disc-like members 8. In this instance, the rotatable support members 8 operate in unison and are provided with an insulating material 9 on the interior faces thereof such that those portions which rotate in an arc-like movement across the ends of the oven section 1 will in effect serve as the end portions of the latter. Also, as best shown in FIGURE 2, there are indicated a plurality of separate spaced apart

chromatograph columns

16, 11, 12, 13, 14- and 15 which in turn are positioned at equal radial distances outwardly from axle 6 and supported between the spaced apart rotatable disc-like members 8. Each of the columns through will of course have suitable end connector means 16 which will permit an easy connection to the tubing or lines which will pass a carrier gas suitable to accommodate a chromatograph sample of the gas to be analyzed in a gas-operation.

While the present drawing indicates the different columns 10 through 15 as being of a similar size and construction, it may be noted that this is merely for illustrative purposes and that such columns will normally be of different sizes and of different configurations and may contain different types of solid adsorbents or of different liquid media on different inert supports, whereby each column is capable of carrying out a specific type of chromatograph analysis on different gas samples. A preferred construction for the multiple column unit also provided for the exchange of difierent columns into the support members 8 whereby they may be easily removed for repair or for substitution purposes. For example, column 12 is shown diagrammatically as being removable from the support members 8 by reason of being in turn supported from small insertable collar or bushing means 17 adapted to be held within notched sections 17' provided from the edges of support discs 8. Set screws or' other locking means not shown may be used to hold the removable portions 17 within the notched sections 17'.

In'the operation of the unit, at the end of any one analysis period it is desired to substitute a new column for a presently used chromatograph column, i.e., column 10 for another type, such as 11, then the side wall portions 1' of the oven chamber may be lifted and the support members 8 rotated whereby the column 10 moves into the position of the column 15, as shown in the present FIGURE 2 while the column 11 then moves into the interior of the heating chamber. After the proper positioning of the substitute chromatograph column, then the hinged oven sections 1 are permitted to be lowered and clamped into place in any suitable manner, even while they are in a heated state. In a similar manner, any other column of the plurality thereof may be rotated into the desired positioning in the oven section for a new analysis procedure by the temporary lifting of the wall sections 1' and the proper rotation of the support members 8.

In FIGURE 3 of the drawing, there is indicated diagrammatically a modified construction and arrangement of the present invention which has an oven section 18 being supported from a suitable bracket means 19 and 20 and a column support plate or member 21 being rotatably mounted on an axle 22. The support member 21 is provided with a plurality of spaced columns such as 23 and 25 which extend perpendicularly therefrom at spaced radial distances which will in turn provide proper positioning within the non-moving oven chamber 18. However, the columns in this instance are provided with tube connector means 24 on the projecting end portions thereof at one end of the heating section and on the exterior face of support disc 21. Thus, the opposing end portion of the oven chamber may be of a fixed permanent construction and the second opposing rotating support member can be eliminated, as compared with the construction shown in FIGURE 1 of the drawing. The substitution of one column for another within the oven section of the unit is, however, carried out in the same manner as that set forth for the embodiment of FIGURES 1 and 2, by utilizing an oven chamber which is provided with hinged or otherwise movable side wall sections permitting their being temporarily raised during that period where one column, such as 23, is replaced with another column such as 25. Again, it may be pointed out that the heating chamber 18, as shown, is merely diagrammatic and that suitable electrical resistance heating coils, or the like, may be provided around the interior wall portions thereof and a suitable power supply source connected therewith in order to provide adjustable heating for such chamber. However, in the interest of simplicity, the electrical heating means and heat control means have not been shown in the present diagrammatic drawing.

In the modified design shown in FIGURE 4 of the drawing, there is indicated an oven unit 26 having movable wall sections 27 and 27', which like the other heating ovens may be suitably provided a heating source not shown. The oven chamber 26 is indicated as being supported by bracket means 28 which in turn extends from a base 29. The latter is shown as being provided with notch or track means 30 to accommodate roller support means 31 on the bottom of a horizontally movable column support means 32. The latter is of an elongated rectangular design adapted to hold a plurality of

chromatograph columns

33, 34, 35 and 36 in a common horizontal plane and at spaced positions which will provide for centering only one of the columns within the interior of the oven section 26 at any one time. The several columns 33 through 36 may extend through opposing spaced apart end support plates, such as 32., or they may be held so as to project outwardly and perpendicularly from the inside face of a single movable support means 32 provided along only one end of the oven chamber 26.

In effecting the substitution of one chamber for another in the heating chamber 26, the

wall sections

27 and 27 shall be temporarily raised or otherwise moved from between the spaced apart columns whereby the lateral or translative movement of the support means 32 with respect to the oven 26 will cause the removal of one column and the substitution of another. After the proper centering of the replacement column within the oven section 26, the wall sections 27 and 27' may be dropped to their closed positions and clamped or otherwise held in place during the period of the next gas analysis procedure.

Again it may be pointed out, that the various columns 33 through 36 may be of entirely different sizes and configurations, or they contain diflerent types of solid adsorbents or liquid film materials on suitable inert mediums whereby entirely different gas analysis procedures may be carried outwith each of the separate column sections. As with the other previously described embodiments, there is no need to wait for an oven chamber cooling off period to effect a substitution of columns inasmuch as all that is required for the change is the rapid lifting of the movable Wall sections, the disconnection of end connector means for the used column section, and the connecting of the gas lines to the replacement column section.

In each of the diagrammatic embodiments of the accompanying drawing there have been shown single coils as providing the various different chromatograph columns for placement in the heating section of the unit; however, it may be noted that many of the modern type chromatograph units make use of dual coil arrangements to serve as any one column in a gas analysis procedure. Thus, it is not intended to limit the present improved multiple column construction and arrangement to the use of single coils for each column, inasmuch as parallel coil type columns may readily be provided for and embodied into the present multiple column concept. In other words, dual column arrangements may be provided for within each oven section at any one time and for any one gas analysis procedure. Also, the column ends and gas line connector means may be provided to terminate exteriorly of one support member or at one manifold means at one end of the oven section or, in an alternative manner, there may be connections to the separate ends of the coils or columns from the opposing ends of the oven section and exteriorly of spaced apart support members or manifold means.

I claim as my invention:

1. A multiple column heating unit providing for the selective insertion of one chromatograph column of a plurality thereof into the oven portion of the unit, which comprises in combination, an elongated oven chamber having a heat supply source for heating a column therein, elongated movable wall portions for such chamber providing for the replacement of a column therein, a plurality of columns extending from end mounting means, with the latter being positioned in combination with said oven chamber to translate with respect thereto and in turn permit any one of said plurality of columns to be positioned interiorly within said oven chamber upon temporarily moving aside said wall portions of said chamber, and attachment means at the ends of each of said plurality of columns for the connection thereof to a gas supply means.

2. The multiple column heating unit of claim 1 further characterized in that the columns comprise more than one size and type where-by the plurality thereof for said unit provide for a rapid change over of columns to permit a different gas analysis utilizing the same heated oven chamber.

3. The multiple column heating unit of claim 1 further characterized in that said oven chamber has opposing hinged wall sections whereby there may be lateral removal and insertion of one column for another within said chamber.

4. The multiple column heating unit of claim 1 further characterized in that said plurality of columns are mounted perpendicularly outwardly from at least one rotating disc-like support member at equal distances from the center of rotation thereof, with such distances providing for the locating of each of the columns interiorly within a fixedly positioned oven chamber, whereby upon the temporary removal of oven chamber wall sections and upon the rotation of the support means there will be the removal of one column out of said oven chamber and the placement of a different column into the interior thereof.

5. The multiple heating unit of claim 4 still further characterized in that the plurality of said columns being supported from the rotating support means have their end sections terminating exteriorly of the latter at one end of the oven chamber.

6. The multiple column heating unit of claim 4 still further characterized in that there are two spaced apart rotatable disc-like support means for said columns and such means are positioned to provide end closures for the oven chamber while being movable across each end and said plurality of columns extend longitudinally between said two opposing rotatable support means with end connecting means provided externally of the opposing support means.

7. The multiple heating column of claim 1 further characterized in that said end mounting means holding said plurality of columns is of a rectangular configuration with said columns being supported therefrom in a spaced parallel arrangement and said end mounting means has movable supporting means arranged to move the mounting means across at least one end portion of said oven chamber, such that upon the temporary lifting of wall sections of the latter there may be a removal of one column and the insertion of a different column within the oven chamber of the unit.

References Cited UNITED STATES PATENTS 1,966,949 7/1934 Goldstein 2l9-385 2,234,499 3/1941 McAllister 23-254 3,139,745 7/1964 Sievers et al. 73-23.1 3,201,921 8/1965 Heyes 386 XR 3,213,596 10/1965 Gill 73-23.1 XR 3,248,517 4/1966 Vranken 219-388 XR 3,290,482 12/1966 Dodd et a1 73-2311 XR FREDERICK L. MATTESON, JR., Primary Examiner. A D. HERRMANN, Assistant Examiner.