WO1991014490A1 - Compresseur a suspension, appareil pour diriger le compresseur et methode pour tasser la boue dans la colonne - Google Patents

Compresseur a suspension, appareil pour diriger le compresseur et methode pour tasser la boue dans la colonne Download PDF

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Publication number
WO1991014490A1
WO1991014490A1 PCT/US1991/001990 US9101990W WO9114490A1 WO 1991014490 A1 WO1991014490 A1 WO 1991014490A1 US 9101990 W US9101990 W US 9101990W WO 9114490 A1 WO9114490 A1 WO 9114490A1
Authority
WO
WIPO (PCT)
Prior art keywords
column
slurry
compressor
adapter
chromatographic column
Prior art date
Application number
PCT/US1991/001990
Other languages
English (en)
Inventor
Yehuda Shalon
Original Assignee
Ht Chemicals Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ht Chemicals Inc. filed Critical Ht Chemicals Inc.
Publication of WO1991014490A1 publication Critical patent/WO1991014490A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • B01D15/206—Packing or coating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/56—Packing methods or coating methods
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/52—Physical parameters
    • G01N2030/522—Physical parameters pressure
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/56—Packing methods or coating methods
    • G01N2030/562—Packing methods or coating methods packing
    • G01N2030/565—Packing methods or coating methods packing slurry packing

Definitions

  • the present invention relates to the field of liquid chromotagraph .
  • the present invention is directed to a an improved apparatus for use in obtaining the high and uniformly pressurized slurry beds employed in present liquid chromatography columns, as well as a method for achieving such uniformly packed columns.
  • Chromatography is a separation method whereby individual chemical compounds which were originally present in a mixture are resolved from each other by the selective process of distribution between heterogeneous phases.
  • the distribution of chemical species to be separated occurs in a dynamic process between a mobile phase and a stationary phase.
  • the stationary phase or the column packing material, usually has a relatively large surface area through which the mobile phase is allowed to flow.
  • the chemical nature of the stationary phase exercises the primary control over the separation process. The greater the affinity of a particular chemical compound for the stationary phase, the longer it will be maintained in the system.
  • the mobile phase can be either gas or liquid; correspondingly, the methods are referred to as gas chromatography and liquid chromatography.
  • Chromatography has been used primarily as a separation and isolation method, and is often intended to separate many mixture components in a single-step procedure. Chromatographic methods can be applied to a very wide concentration range; from commercial scale quantities (gram-kilogram range) all the way to analytical
  • Chromatographic separations are based upon the physicochemical principals , of adsorption and partion, and, conversely, these and related fxindamental physicochemical phenomena can be studied by high precision chromatography of model systems.
  • the mobile phase may be perculated through the column at atmospheric pressure, by means of gravity, or under more contemporary procedures, through the pressure generated by smaller and smaller particles of the packing media.
  • High pressure pumps which can generate up to several thousand atmospheres of inlet pressure are often used.
  • HPLC high pressure liquid chromatography
  • Preparative high pressure liquid chromatography is a process in which one applies a mixture of a compound in solution and in its mobile phase where, by virtue of the selection of the components of the column packing material, the column will retain the various and select components of the mixture for that length of time which causes its select components to be eluted discretely for separate collection as individual components and as purified elements.
  • preparative HPLC the separation and purification is in larger quantities than in analytical HPLC.
  • HPLC high pressure liquid chromatography
  • the columns used in chromatographic analysis are generally fabricated of metal, such as stainless steel, and function to separate various chemicals (for analysis or use) that pass through the columns at pressures that range from up to 2000 to 4000 psi.
  • the chemicals passed through the absorbent bed are separated into their constituents so that the various desired elements can be obtained, or an analysis of the chemical passing through the column can be performed.
  • a critical feature in ensuring the proper operation of such columns relates to the degree and uniformity of compactness of the packed absorbent bed contained within the column.
  • This slurry packing must be maintained at a very high pressure, and at a uniform density, in order to achieve the most efficient and effective results during the chromatographic procedure.
  • the present invention relates to the configuration and structure of columns for use in preparative liquid chromatography.
  • the present invention also relates to an apparatus for ensuring the uniformity of slurry and pressure applied to such a column while at the same time minimizing and/or preventing leakage of particles past the pressure applying mechanism.
  • the slurry compressor of the present application facilitates obtaining a homogeneous absorbent packed bed in liquid chromatography columns, thus improving the efficiency of the columns and increasing the accuracy of the results obtained thereby.
  • the particularly designed and styled compressor of the instant application is particularly designed to eliminate the leakage of particles past the compressor while at the same time enabling very high and uniform pressures and densities to be achieved.
  • the present invention also relates to an adapter or tool which facilitates and/or enables insertion of the inventive slurry compressor into the column without damaging the compressor or the sealing members carried thereby.
  • the present invention also relates to a method of mixing the slurry prior to packing to enhance its separating qualities.
  • the instant slurry compressor is an improvement over the compressor disclosed in U.S. Patent No. 4,675,105 (MARTIN et al.) entitled "System for Obtaining a Homogeneous Absorbent Bed in a Chromatographic Column".
  • the present invention also relates to a handled straight adapter for use between two chromatographic columns that facilitates packing of the working column from an attached reservoir column.
  • the instant handled straight adapter is an improvement over the adapter disclosed in U.S. Patent No. 4,719,011 (SHALON et al.) entitled "High Pressure Liquid Chromatography Columns”.
  • MARTIN et al. patent a slurry compressor is disclosed for obtaining a homogeneous absorbent bed in a liquid chromatographic column.
  • the compressor includes a solid, shaped compressor member having external dimensions only very slightly less than the internal dimensions of the column in which the bed of particles being compressed is contained.
  • the compressor includes an innermost portion which, in use, is in contact with the particles within the column and an outermost portion integrally connected to the innermost portion.
  • the innermost portion is a solid segment while the outermost portion is formed with a hollowed interior forming a walled structure extending rearwardly from the solid portion.
  • the walled structure of the outermost portion is shaped to flare slightly outwardly from the inner portion in order to tightly and sealingly contact the inner wall surface of the associated reservoir column.
  • the flared wall portion acts as a seal, preventing the slurry from leaking past the compressor element.
  • Also provided in the present invention is a tool and adaptor element that cooperates with the slurry compressor and with the column for enabling the slurry compressor to be quickly and efficiently inserted into the liquid chromatographic column without damaging any portion thereof.
  • the present invention thus relates to an improved slurry compressor having an improved resilient sealing means, to an adaptor tool for inserting the compressor into the chromatographic column without damaging any portion thereof, to a method of mixing the slurry prior to compression thereof, as well as to an adaptor element with outwardly extending handles.
  • the above-mentioned modular liquid chromatography system has been quite successful in providing a wide range of column widths and lengths by virtue of the use of various types of adapters, such as straight adapters for connecting columns of equal diameter and conical or tapered adapters for connecting columns having different diameters.
  • the present invention solves this problem by providing an adapter having handles integrally attached thereto to facilitate removal of the adapter from the column.
  • the present invention solves this problem by providing an adapter having handles attached integrally thereto to facilitate restraining the upward expansion of the pressurized slurry bed from the working column. This permits removal of the reservoir column from the working column and removal, as by a wire knife or other means, of the extra packing media from the working column as it expands therefrom.
  • the use of the instant handled straight adapter which is used to connect both columns prevents damage to the prepared packed bed within the working column.
  • the present invention also relates to an improved straight adapter for coupling two column portions together.
  • the improved adapter of the present invention is provided with handles so that during use (i.e., filling and packing of the column) the column can be stabilized by being attached to a support structure via the handles attached to the adapter, and upon disassembly of the columns, because of the handles provided on the adapter, the prepared packed column bed is not damaged. Since the filling, assembly, and pressurization (packing) of the column takes some period of time, the filling material (slurry mixture) often tends to undesirably settle out during the filling process.
  • a method for filling and preparing chromatographic columns is set forth that eliminates such problems and enables the columns to be filled in such a manner that the contents of the slurry bed therein remain uniform. This has made the slurry packed columns much more efficient and effective in being utilized for preparatory chromatography.
  • the double sealed slurry compressor with the flared end up is inserted on the top of the reservoir column with the aid of the compressor adapter. Once the compressor is in place the adapter is removed form the reservoir column. The top of the reservoir column is now sealed with a large O-ring and an end plate. The end plate is mounted securely with bolts and nuts. This endplate will later be connected to the packing instrument.
  • the mixed slurry is then poured into the assembled columns.
  • the assembly is not filled totally, thus a substantial amount is left empty, which will create an air bubble in the assembly.
  • the working column is now sealed with a large and small O- ring, a bed support frit, a disperser frit, and an end plate and tightened with bolts and nuts.
  • the assembled columns are now sealed and shaken or mixed so that the contents (i.e., the slurry mixture) are mixed so that the air bubbles contained within the column will serve as a mixture device to maintain the homogeneous nature of the slurry and prevent settling out of the slurry components prior to the application of pressure to the slurry filled assembly.
  • the slurry can be pressurized to a uniform and high pressure and density by applying pressure to the instant improved double sealed slurry compressor, which is positioned on top of the reservoir column which is attached to the packing instrument.
  • the procedure of removing the reservoir column from the working column can be performed only after the pressure is released.
  • the invention involves a slurry compressor for use in a chromatographic column adapted to contain a bed of particles comprising a slurry, the compressor being a shaped member having an inner portion and an outer portion.
  • the inner portion is a solid segment that includes a generally planar surface which is adapted to contact the slurry, while the outer portion is a hollowed interior defined by a walled structure extending from the solid segment forming the inner portion.
  • the inner portion includes an annular groove positioned intermediate the generally planar surface and the outer portion and the groove comprises means for receiving a resilient means adapted to seal an interface of a column and the compressor.
  • the compressor further including resilient means for sealing that is positioned within the groove, and comprises a resilient O-ring.
  • the groove further includes means for receiving at least one backup spacer member.
  • the structure includes walls which flare slightly outwardly from the inner portion.
  • the slurry compressor is formed of a polymer and the inner and outer portions of the slurry compressor are integrally connected.
  • the resilient sealing means is a resilient O-ring and includes at least one backup spacer element positioned within the groove.
  • the backup spacer element is positioned between the O-ring and the generally planar surface and comprises a split ring of glass loaded polymer. Two backup spacer elements can be positioned in the groove with the O-ring positioned between the spacer elements.
  • the O-ring, spacer element and the wall structure each comprise means for sealing an annular space between the column and the compressor.
  • the invention also relates to an adapter comprising means for engaging the column opening and means for receiving and guiding the compressor into the column opening.
  • the invention relates to a receiving and guiding means that comprises a tapering funnel member and an engaging means that comprises a support element engaging the column opening with a first flange engaging a top wall surface of the column opening and a second flange engaging a side wall surface of the column opening.
  • the receiving and guiding means comprises a hollow tapering funnel member and the engaging means comprises a flanged hollow member.
  • the invention also includes a liquid chromatography column in combination with the adapter apparatus which includes a hollow tapering funnel member and a flanged hollow member.
  • the invention further sets forth an apparatus for obtaining a slurry comprising a homogeneous absorbent bed of particles in a chromatographic column under pressure.
  • the apparatus includes a slurry compressor including a first portion comprising a slurry contacting face and a second portion comprising a pressure receiving surface with I -
  • the second sealing means comprises a walled structure flaring outwardly from the first portion and the resilient means comprises a resilient O-ring positioned within an annular groove of the first portion.
  • the resilient means comprises a resilient O-ring and a backup spacer element positioned within an annular groove of the first portion.
  • the backup spacer element comprises a flat, annular split-ring element.
  • the invention relates to an adapter element for use between two terminally flanged columns of a chromatography assembly with the columns adapted to be assembled with the adapter element positioned between them.
  • the adapter element is an annular member having an exterior periphery and an internal aperture, the internal aperture defined by a diameter which is generally similar to the internal diameter of the column and means for stabilizing the adapter during disassembly of the columns and attached to the exterior periphery of the annular member.
  • the stabilizing means comprises a plurality of handles extending outwardly from the annular member.
  • the stabilizing means further comprises means for securing the adapter to a support structure.
  • the handles comprise means for preventing a compressed slurry within a chromatographic column from expanding out of the column.
  • the handles also comprise means for attaching the assembly to a stabilizing support structure.
  • the handles can include a reinforcing rib and clamping means can be attached to the handles.
  • the invention further involves a method of packing a chromatographic column with a slurry.
  • the method comprising the steps of inserting a slurry compressor element into a reservoir column, assembling the reservoir column to a column to be packed, pouring a slurry into the assembled columns, shaking the assembled columns with the slurry therein and uniformly compressing the slurry within the assembled columns by applying pressure to the slurry in the working column via the compressor element positioned within the reservoir column.
  • the method further includes the step of disassembling the reservoir column from the packed column containing the slurry and the step of inserting a slurry compressor into a reservoir column includes installing an O-ring and a backup member in a groove of the slurry compressor element.
  • the step of assembling the reservoir column and the column to be packed includes positioning a handled straight adapter between the columns.
  • the step of assembling the reservoir column to the column to be packed further includes attaching the handles of the handled straight adapter to a support surface.
  • the step of disassembling the reservoir from the packed column includes loosening the reservoir column assembly bolts and cutting through the packed slurry.
  • the step of disassembling the reservoir column from the packed column includes the step of removing the handled adapter from the opening of the packed column.
  • the step of disassembling the reservoir column from the packed column includes cutting the packed slurry bed level with the column opening, after removal of the straight handled adapter.
  • Fig. 1 is a perspective view of the slurry compressor of this invention
  • Fig. 2 is an end view of the slurry compressor of Fig. 1, directed at the outer or rear portion thereof;
  • Fig. 3 is an end view of the slurry compressor of Fig.
  • FIG. 4 is a sectional view of the compressor of the present invention, taken along the section line 4-4 of Fig.
  • FIG. 5 is plan view of one end of the compressor adapter or tool of the present invention that is used to insert the slurry compressor into the reservoir column;
  • Fig. 6 is a cutaway sectional - and side view of the compressor adapter of Figure 5;
  • Fig. 7 is a plan view of one end of the handled straight adapter/connector of the present invention.
  • Fig. 8 is a side sectional view of the handled straight adapter/connector of Fig. 7, taken along section lines 8-8 therein;
  • Fig. 9 is a sectional view of the handled adapter/connector of Figs. 7 and 8, installed between two chromatographic columns according to one feature of the present invention.
  • Fig. 10 is a sectional view of the compressor adapter mounted to a column with a slurry compressor being inserted to the column via the adapter.
  • a slurry compressor 10 comprising a generally cylindrically shaped element 10 having a first portion, referenced as the inner portion, and terminating in a planar front surface 18, and a second outer or rear portion which is opposite to and integrally joined with the inner portion.
  • the inner portion is a solid cylindrical member 12, defined by a first planar surface 18, which, in H use, is adapted to be driven by hydraulic pressure or other means against a slurry which usually comprises a bed of silica particles.
  • the opposite end surface 22 of the inner portion 12 of the compressor 10 is seen to be the bottom surface of a generally hollow walled structure which is fabricated integrally with the inner portion.
  • the outer or rear portion of the compressor comprises the circumferentially arranged, generally frustoconical flexible wall 14, and the surface 22, which together define a hollow recess 16 in the back end of the compressor element.
  • the back end of the compressor element is the end to which a hydraulic (or other) force is applied to compress the slurry which is in contact with the surface 18 of the inner portion of the compressor element.
  • the size of the compressor element at the inner portion and at the surface 18 is selected to be very slightly less than the inner diameter of the chromatographic column, (e.g., a reservoir chromatographic column) within which it is to be employed. As seen in the drawings, and most particularly in Fig.
  • the circumferential wall 14 flares slightly outwardly from the body of the compressor in a radial manner so as to provide a tight seal against the inner wall surface of the column.
  • the use of tapered walls having a dimension such as to abut tightly, by virtue of their resilience, against the inner surface of the column, is designed to prevent the leakage of slurry past the compressor element. Further disclosure of the structure and use of a predecessor slurry compressor element is contained in the above-referenced patent to Martin et al. (U.S. Patent 4,675,105), the entire disclosure of which is expressly incorporated herein by reference.
  • the compressor element 10 is provided with an annular, generally rectangular in cross- section groove 22, adjacent surface 18.
  • the annular groove 22 is inscribed in the circumferential wall of the compressor element inner portion and is generally parallel to the bottom surface thereof.
  • a flexible O-ring sealing member 26 can be disposed within the groove 22 to serve to resiliently abut against the walls of the chromatographic column 60, and to act as a seal to prevent any of the slurry from leaking past the compressor element 10.
  • either one or two split ring spacer elements 24 can be provided. If two such rings are provided, one would be positioned on either side of the flexible O-ring within the groove 22. If only one split ring spacer element 24 is provided, it should be located on that side of the flexible O-ring opposite to which a (hydraulic) pressure is applied. Thus, if only one split ring spacer element is provided, it would be located relative to the O-ring and the bottom surface 18 as shown in the sectional view of the Fig. 4. While only one split ring spacer/back-up element is shown in Fig. 4, it is explicitly within the scope and contemplation of the invention that two (or more, for that matter) back-up spacer rings 24 can be utilized herein, in which case one would be positioned on either side of the resilient O-ring 26.
  • the split ring backup spacer elements 24 are fabricated of a glass loaded polymer material so as to provide additional structural rigidity and support for the resilient O-ring 26, which is formed, e.g., of a suitable elastomer.
  • the outer diameters of the O-ring 26 and the split ring backup spacer 24 are substantially the same. Both of these elements provide additional sealing for the l (
  • the O-ring 26, seated within the groove 22 must seal perfectly with the inner walls of the chromatographic reservoir column 60.
  • Chromatographic columns are generally made of stainless steel and the interior surfaces of these columns are finished to a very high degree of smoothness.
  • the column wall surface might be marred by imperfections.
  • the compressor body itself is very slightly smaller that the column into which it is to be inserted; however, the O-ring, in order to function properly, must be slightly larger then the column, and must as a result, be inserted into the column with a great deal of pressure.
  • Fig. 6 essentially acts as a funnel to assist and facilitate the insertion of the compressor element shown in Figs. 1-3 into the chromatographic reservoir column, as shown in Fig. 4, without causing any damage to the resilient surface of the O-ring thereof.
  • the adapter As shown in Figs. 5 and 6, the adapter, generally designated as 80, is formed of stainless steel or other similar durable and smooth material.
  • the top portion (as used) of the adapter member is a generally hollow cylindrical component 84 having frustoconical inner walls with a slight interior taper, as shown at 86, and an axially extended, generally annular flange member 82 connected to the walls 84.
  • a second, relatively short, upstanding cylindrical member 90 is provided.
  • This member 90 is also hollow and acts as a continuation of the funnel shaped component 84, as shown in the partial sectional view of Fig. 6. As noted above, and as seen in the partial section view of Fig.
  • the walls 84 of the interior of the cylinder taper inwardly from a somewhat wider opening at the mouth outer portion 92, to a slightly narrower portion extending inwardly from the inner surface of the adapter. Beyond the tapered portion 86, the adapter has a rounded transition portion 88. The wall then extends I I into the uniform dimensioned entrance portion which comprises the interior of the upstanding member 90.
  • the member 90 and the supporting flange 82 are placed over the inlet portion of a stainless steel chromatographic reservoir column.
  • the compressor with the split ring spacer back ⁇ up member 24 and resilient O-ring 26 positioned within the groove 22, are then inserted into the outer portion or mouth of the funnel 86.
  • the compressor can be safely and without damage inserted into the column 60 to attain the position of Fig. 4.
  • the degree of taper of the walls 86 is not critical, but should be fairly slight and should also be adequate to enable the compressor to be pushed therethrough and into the column inlet.
  • the shape and structure of the tool/adapter 80 is such as to prevent any damage occurring to the resilient ring of the compressor element as it is being inserted into the column.
  • Fig. 10 shows the adapter 80 positioned with the wide portion of the funnel section 84, 86 facing upwardly over the inlet mouth (or top) of a reservoir column 60 having a flange 112 positioned there at. Also shown is with a slurry compressor 10 (with the resilient O-ring 26 and split ring backup spacer member 24 positioned in the groove 22) positioned with the flared portion facing upwardly, at the inlet of the adapter.
  • the adapter flange 82 is positioned in overlying relation to the column flange 112.
  • the above- mentioned patent discloses and describes various forms of adapters including a straight adapter, a frit adapter and a tapered and/or conical adapter.
  • the present invention also involves an improved handled straight adapter for use in packing chromatographic columns of the type disclosed and discussed in the above-mentioned SHALON et al. patent.
  • an improved handled straight adapter designed to enable efficient packing of chromatographic columns from attached reservoir columns without damaging the compressed slurry bed contained therein, is provided by the present invention.
  • the improved straight adapter of the invention is illustrated in Figs. 7-9. With particular reference to Fig. 7, an end view of the adapter 100 is shown.
  • the adapter comprises an annular section 102 provided with a plurality of bolt holes 104 spaced thereabout. These holes, as can be seen in Fig. 9, are engaged by bolts 118 which also pass through the opposed flanges 112, 112* of the working column to be packed 60', and the reservoir column 60, which are to be joined through the intermediary of the herein described adapter 100.
  • an upstanding flange 108 Adjacent to the interior annular aperture 110, there is provided, on one side, an upstanding flange 108 as the interior boundary surface of the straight adapter.
  • this upstanding flange 108 is seated within a correspondingly provided annular groove in the end face of the column 60' to be packed.
  • the use of this annular flange 108 provides the interior surface of the joined columns with an uninterrupted smooth surface.
  • the other side of the straight adapter is provided with a flat surface 109.
  • outwardly extending, elongated generally flat handles 106 are provided. These handles, attached to the straight adapter, assist in the stabilization of the connected reservoir and packing column during the assembly thereof.
  • handles and the attachment of these handles to any convenient support structure also facilitates the shaking and agitation of the connected columns to ensure that the homogeneous nature of the slurry is maintained during the filling process before packing the slurry.
  • the flat surface 109 of the straight adapter enables straight and even cutting of the packing media with a wide knife or a similar tool across the inner diameter above the packed column.
  • the straight adapter with handles also assists in the removal of the adapter from the columns after the slurry has already been compressed within the connected reservoir and working columns.
  • the handles are provided with £ ⁇ a somewhat tapered cross-sectional area, and the central portion thereof can be provided with a rib (not shown) so as to provide additional strength to the handles. While this ribbed structure contributes to the strength of the handles, it is not an essential part of the handle structure per se. In particular, and if necessary, any other conventional reinforcing mechanism to ensure that the handles have the adequate strength for the uses for which they are designed can also be utilized therein. Since one of the functions of the handles when used between attached reservoir and packing columns is to be attached to an appropriate support structure, various attachment means can be included in the structure of the handles.
  • the straight handled adapter shown in the drawings is noted to show a plurality of apertures through the outwardly extending portions thereof.
  • the locations of these apertures are merely exemplary.
  • the positioning of the apertures and/or of additional structure that can be utilized to provide a support for appropriate securing mechanisms that could be attached to the adapter, and the columns to which it is assembled, to in turn enable the adapter to be supported, can be modified as needed.
  • these apertures can readily be eliminated, and other conventional means can be used for attaching the handled adapter to an appropriately located support structure.
  • Fig. 9 shows the improved handled straight adapter joining a reservoir column 60 to a chromatographic column 60' to be packed with a slurry bed.
  • Each column is provided with a flange member 112, 112• attached to the outer surface of the end portion thereof.
  • Each of the flange members has an annular recess in an end surface thereof for receiving therein a sealing O-ring 116.
  • the 0-rings 116 abut opposite sides of the straight adapter 102, and act as seals between these components.
  • the two flanges are assembled face-to- face, and nut and bolt assemblies 118 and 120 are inserted into the appropriate holes positioned about the periphery of the annular flanges in an array corresponding to the holes 104 illustrated in Fig. 7 for the straight adapter. As all of these holes are aligned, the bolts 118 and mating nuts 120 can be inserted and tightened down to form a single unitary chromatographic column.
  • the flange 108 of the straight adapter in its use orientation, can be clearly seen.
  • the handles of the straight adapter extend outwardly beyond the flanges 112 and are visible when the mechanism is in use.
  • the handles enable the joined columns to be secured to an appropriately positioned support structure (not shown).
  • the support structure utilized can be, e.g., a column support stand specifically designed to support a column or columns or any other support structure that is positioned with respect to the joined columns so as to enable the columns to be secured thereto.
  • another significant feature of the present invention is utilized.
  • the slurry in the column is mixed by tilting and/or shaking the assembled columns in any convenient and conventional manner.
  • any form of mechanical agitating or mixing device can be used, or depending on the size of the columns they can be mixed by merely being shaken up and down or in any other fashion to enable the air bubbles therein to mix and maintain the homogeneous nature of the slurry within the column.
  • Substantially enhanced results are obtained by utilizing a column wherein the slurry therein has been mixed by mechanical agitation or by any other mechanism so as to ensure that the homogeneous nature -?3 of the slurry contained within the column is maintained. After the slurry is mixed and the pressure supplying mechanism is attached to the column by means of provided line fittings, the slurry can then be pressurized to form a solid bed.
  • the straight handled adapter of the present invention plays a major role in ensuring the disassembly of the reservoir column from the packed column without disturbing the condition of the packed slurry bed within the packed column.
  • a major function of the enhanced handled straight adapter is to assist in the stabilizing of the silica slurry in the column during the separation of the reservoir column from the working column after it has been packed.
  • the working column Prior to the packing of the working column, the working column is attached, via the flanges 112, 112', to a reservoir column.
  • the packing media is inserted through the reservoir column and is compressed downwardly into the working column by use of the slurry compressor. After the working column is fully loaded with compressed silica, the reservoir column is removed. Because, during the packing process, the packing media slurry is compressed under great pressure, upon removal of the reservoir column, the packing media naturally tends to expand outwardly from the mouth of the packed column.
  • the straight adapter with the handles as shown herein, upon removal of the reservoir column, the expanding packing media out of the working column can first be shaved off by the use of a straight edge wire or similar implement.
  • the handles 106 are generally secured, as by rings or clamps, to any convenient support structure so as to provide further stability to the column itself.
  • the disassembly of the reservoir column from the packed column according to the invention is performed in the following manner. First, after the pressure is released, the majority of the nuts and bolts connecting the reservoir column to the working column, i.e., packed column, are removed. Two opposite bolts are allowed to remain and these are loosened so that a cutting wire or other implement, as noted above, can be inserted, and the slurry bed within the still-joined columns can be cut through from one end to the other. Thereafter, the last two nuts and bolts can be removed, after which the reservoir column can (and should) be removed from the column containing the packed slurry bed. At this point, the straight handled adapter is still positioned on top of the packed slurry within the column that has been packed under pressure.
  • a plate is then placed on top of the slurry, within the central aperture of the handled adapter.
  • the plate and straight adapter are then held securely by applying pressure downwardly to prevent the adapter and plate from lifting up due to the expansion of the compressed slurry thereunder.
  • the straight adapter can then be detached from whatever support structure it was attached to prior to packing of the slurry within the chromatographic working column; and, thereafter, the straight adapter and plate can be carefully removed, making certain not to destroy or in any way mar the finish of the packed bed.
  • a straight edge sharp knife or other appropriate implement can then be used to cut the packed bed flat at the height of the flange in the mouth of the packed column.
  • the handled straight adapter of the present invention enables the columns to be disassembled without damaging the packed slurry therein and thus contributes to the efficient packing of columns. It also enables the columns to be agitated and mixed to enable the slurry within the columns as it is being inserted therein to be maintained as a homogeneous mixture.
  • the chromatographic columns for which the invention is set forth herein are generally formed of a stainless steel.
  • the compressor element which is the subject of the instant invention can be fabricated. e.g., of a technical grade TFE.
  • the O-ring can be formed, e.g., of a florez material.
  • the split ring spacer backup member can be formed, e.g., of a glass loaded TFE material.
  • the adapter 80 and the straight adapter 102 can each be fabricated, e.g., of stainless steel or aluminum.
  • the above mentioned material of which the various components of the present invention can be fabricated are not intended to be limiting in any manner. Various other, materials with satisfactory properties can be utilized as an alternative herein. The above materials are merely included for the illustrative purposes of showing a particular preferred material of which the components of the present invention can be fabricated. Different materials can obviously be utilized and still remain within the scope of the present invention.

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

Un compresseur à suspension (10), servant à obtenir un lit de boue homogène, pressurisée, tassée et absorbante dans une colonne à chromatographie (60) est décrit. Le compresseur (10) comprend une première partie solide (18) et une seconde partie (14) qui est une structure dotée de parois et légèrement conique solidaire de la première partie (18). Une fente en forme d'anneau (18) est située dans la première section (18) et un joint torique d'étanchéité élastique (26) est placé à l'intérieur de l'anneau (22). Un élément d'écartement en appui à bague à fente (24) peut aussi être placé dans ladite fente pour fournir une étanchéité renforcée afin de prévenir la fuite de particules au-delà de l'élément compresseur (10). Un élément adaptateur (80) devant permettre l'introduction du compresseur (10) dans la colonne (60) sans endommager la surface du joint torique (26) est aussi décrit. Un adaptateur droit à poignées (100) est aussi fourni pour permettre de soutenir la colonne (60) pendant le tassement et de la stabiliser au cours du démantèlement de la colonne (60). Une méthode pour tasser la colonne (60), qui consiste à secouer la colonne remplie de boue (60) avant la pressurisation de ladite colonne (60) est aussi décrite.
PCT/US1991/001990 1990-03-29 1991-03-28 Compresseur a suspension, appareil pour diriger le compresseur et methode pour tasser la boue dans la colonne WO1991014490A1 (fr)

Applications Claiming Priority (2)

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US50112290A 1990-03-29 1990-03-29
US501,122 1990-03-29

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999029389A1 (fr) * 1997-12-10 1999-06-17 Prior Separation Technology Gmbh Procede pour charger l'espace du lit de particules d'un chromatographe
CN103221818A (zh) * 2010-11-29 2013-07-24 通用电气健康护理生物科学股份公司 用于将层析柱的分配器板固定到背板上的方法和装置
US9289699B2 (en) 2009-07-30 2016-03-22 Hoffmann-La Roche Inc. Moveable chromatography column separator
US11241638B2 (en) 2011-02-02 2022-02-08 Hoffmann-La Roche Inc. Chromatography column support

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3487938A (en) * 1968-08-08 1970-01-06 Sondell Research & Dev Co Chromatographic column head space reducer
US4675105A (en) * 1985-03-22 1987-06-23 Ht Chemicals, Inc. System for obtaining a homogeneous absorbent bed in a chromatographic column
US4719011A (en) * 1985-03-22 1988-01-12 H. T. Chemicals, Inc. High pressure liquid chromatography columns

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3487938A (en) * 1968-08-08 1970-01-06 Sondell Research & Dev Co Chromatographic column head space reducer
US4675105A (en) * 1985-03-22 1987-06-23 Ht Chemicals, Inc. System for obtaining a homogeneous absorbent bed in a chromatographic column
US4719011A (en) * 1985-03-22 1988-01-12 H. T. Chemicals, Inc. High pressure liquid chromatography columns

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999029389A1 (fr) * 1997-12-10 1999-06-17 Prior Separation Technology Gmbh Procede pour charger l'espace du lit de particules d'un chromatographe
US9289699B2 (en) 2009-07-30 2016-03-22 Hoffmann-La Roche Inc. Moveable chromatography column separator
US10052567B2 (en) 2009-07-30 2018-08-21 Hoffmann-La Roche Inc. Moveable chromatography column separator
CN103221818A (zh) * 2010-11-29 2013-07-24 通用电气健康护理生物科学股份公司 用于将层析柱的分配器板固定到背板上的方法和装置
CN103221818B (zh) * 2010-11-29 2015-08-05 通用电气健康护理生物科学股份公司 用于将层析柱的分配器板固定到背板上的方法和装置
US11241638B2 (en) 2011-02-02 2022-02-08 Hoffmann-La Roche Inc. Chromatography column support

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