EP2836830A1 - Élément de retenue pour sorbants monolithiques - Google Patents

Élément de retenue pour sorbants monolithiques

Info

Publication number
EP2836830A1
EP2836830A1 EP13712148.9A EP13712148A EP2836830A1 EP 2836830 A1 EP2836830 A1 EP 2836830A1 EP 13712148 A EP13712148 A EP 13712148A EP 2836830 A1 EP2836830 A1 EP 2836830A1
Authority
EP
European Patent Office
Prior art keywords
tube
holder
pressure
monolithic
holder according
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP13712148.9A
Other languages
German (de)
English (en)
Inventor
Karin Cabrera Perez
Klaus Kreher
Willi Neuroth
Michael Ukelis
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
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 Merck Patent GmbH filed Critical Merck Patent GmbH
Priority to EP13712148.9A priority Critical patent/EP2836830A1/fr
Publication of EP2836830A1 publication Critical patent/EP2836830A1/fr
Withdrawn legal-status Critical Current

Links

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
    • 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
    • G01N30/60—Construction of the column
    • G01N30/6047—Construction of the column with supporting means; Holders
    • 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
    • G01N2030/524—Physical parameters structural properties
    • G01N2030/528—Monolithic sorbent material

Definitions

  • the present invention relates to a holder for monolithic
  • Sorbents in which a radial pressure can be exerted over the entire length of the sorbent by means of a tapered tensioning tube.
  • the filler material is filled into a stainless steel or plastic tube with precisely fitting ends. This ensures that the sorbent bed is tight against the jacket of the column and the sorbent particles are distributed homogeneously over the entire cross section of the column.
  • Inorganic or organic monolithic moldings may shrink in their manufacture so that they can not remain in the original form in which they are produced. You must use a new fluid-tight and pressure-resistant
  • Sheath be provided. This is the only way to ensure that sample and eluent are transported exclusively through the sorbent.
  • Monolithic sorbents consist of a porous shaped article, e.g. from silica gel, silica gel-containing materials or organic polymers.
  • Various possibilities for the liquid-tight coating of monolithic sorbents are described in WO 98/59238, EP 1269179 and
  • EP2118646 This includes, for example, a jacket with pressure-resistant plastics, such as PEEK (polyetheretherketone) or fiber reinforced PEEK.
  • PEEK polyetheretherketone
  • fiber reinforced PEEK fiber reinforced PEEK
  • chromatographic properties show monolithic sorbents with a bimodal pore system with macropores (Through pores) on the one hand and mesopores in the skeleton on the other hand.
  • the macroporous size determines the permeability or the flow resistance and respectively the column back pressure.
  • the mesopores serve the
  • the macro pore diameter also determines the
  • a monolithic column with a column diameter of 4.6 mm and a diameter of 2 ⁇ m macropores has a back pressure of about 25-30 bars at a flow of 2 mL / min (ACN / water; 60/40) while the column has the smaller macropores have a back pressure of about 50-70 bar under the same chromatographic conditions.
  • the subject of the present invention is therefore at least a holder for holding a monolithic chromatography column
  • a clamping tube whose inner diameter is constant and the outer diameter grows uniformly to a point between the two ends, to one end or both ends and having one or more slots in the longitudinal direction of the tube -
  • a pressure sleeve consisting of a tube whose inner diameter grows uniformly from one end to the other end and the outside has at least one flange or groove
  • the clamping device consists of two screw parts whose inner diameter is larger than that
  • the holder is made of stainless steel.
  • the outer diameter of the tensioning tube increases toward the center.
  • the holder has two
  • the tensioning tube has 6 to 12 slots.
  • the slope of the lateral surface of the prestressing tube is between 1:60 and 1:40.
  • the tensioning device is actuated mechanically, hydraulically, pneumatically or electromechanically. It is particularly preferably operated mechanically.
  • the subject of the present invention is also a separating device at least consisting of a holder according to the invention and a monolithic chromatography column. In a preferred embodiment, the monolithic
  • the PEEK or PPS can be combined with e.g. Coal or glass fibers should be fiber reinforced or not.
  • the monolithic sorbent of the chromatography column has a diameter between 1 mm and 25 mm.
  • the present invention also relates to the use of a holder according to the invention or the invention
  • Separating device for the chromatographic separation of at least two substances.
  • Figure 1 shows a schematic possible outline of tensioning tubes.
  • Figure 2 shows schematically a pressure sleeve (without flange or groove).
  • Figure 3 shows a holder according to the invention with inserted chromatography column.
  • FIG. 4 to 9 show the individual components of the
  • a tube is an elongated hollow body whose length is generally much larger than its diameter. Tubes typically have a circular cross section at least in the cavity. According to the invention tubes can consist of a workpiece or of two or more workpieces, which can be joined together to form a tube. For example, according to the invention, a tube can also consist of two half shells, which can be joined together to form a tube.
  • the tubes used according to the invention, such as the tensioning tube or the pressure sleeve preferably consist of a workpiece.
  • the core of the holder according to the invention is the clamping tube. It is designed so that the monolithic column can be inserted into the clamping tube. Preferably, the monolithic column should fit accurately into the clamping tube can be inserted. That means that
  • the tensioning tube may consist of one or more parts, which together form a tube.
  • the tension tube has at least the length of the monolithic sorbent for which it is intended to be sheathed.
  • the clamping tube has a cavity with a circular cross-section.
  • the wall of the clamping tube is circular in shape.
  • the inner diameter of the clamping tube is the same over the entire tube length. This means that the clamping tube has a cylindrical cavity.
  • the outer diameter of the tension tube either from both sides of the tension tube to a point between the ends
  • the increase in the diameter of the tensioning tube can be represented by the slope of the lateral surface of a straight cone.
  • the slope should be at least 1:75. Typically, it is no larger than 1: 5.
  • Preferred values are in the range between 1:60 and 1:40, more preferably 1:50. This means over a length of 50 cm, the diameter of the tensioning tube particularly preferably increases by about 2 cm (the diameter of a straight cone is twice the radius of the cone at this point).
  • the tension tube has at least one slot in the longitudinal direction of the tube. These slots may be run the full length of the tube so that the tube is divided by the slots into two or more pieces.
  • the end may be run the full length of the tube so that the tube is divided by the slots into two or more pieces.
  • a slot is according to the invention in the longitudinal direction of the tube
  • This breakthrough is designed so that when it is made starting from a one-piece clamping tube without slots, not only by cutting the wall of the clamping tube takes place but at the same time Material discharge takes place. That means the slits in the wall of the
  • Clamping tube are not only longitudinal cracks but longitudinal holes in which a small part of the wall of the clamping tube was removed in relation to the wall of the clamping tube without slots. Looking at the circular cross-section of the tensioning tube, there are typically 5 to 15% of the cross section of slot and the remainder of wall over the sum of all the slots.
  • the tension tube has 6 to 12 slots. It has been found that in this way a tension tube is formed, which can be pressed evenly and radially on a monolithic sorbent located in the pipe by its uniform inner diameter and the slots located in the pipe wall. Through the slots, the inner diameter of the clamping tube can be adapted exactly to the outer diameter of the sorbent. By pressing the clamping tube on the monolithic sorbent narrow the slots, which leads to a reduction of the clamping tube diameter. This will do that
  • a pressure sleeve consists of a tube whose inner diameter grows uniformly from one end to the other end and which has at least one flange or a groove on the outside.
  • a flange means an annular
  • Thickening or a waistband and similar thickening e.g. in the form of individual knobs are annularly mounted around the pressure sleeve around.
  • the flange is preferably worked integrally with the pressure sleeve, but can also be subsequently glued, screwed or otherwise secured to the pressure sleeve.
  • a groove is
  • Simplification is here a flange or a groove not shown.
  • Figure 4 shows a possible embodiment of a pressure sleeve with bottle / groove.
  • the inner diameter of the pressure sleeve is constructive on the
  • Compression sleeves is not critical.
  • the one or more compression sleeves used should encompass the entire length of the tension tube. In this way, an ideal pressure transfer to the clamping column is guaranteed.
  • the compression sleeves on both sides of the tension tube over, so that column end pieces with filters,
  • Precolumns, perforated plates or the like can be connected to the compression sleeves.
  • Such end pieces correspond to the
  • the pressure sleeves can be provided with corresponding internal or external threads for connecting the end pieces.
  • the pressure sleeves can be provided with threads or plug-in devices for connection of the solvent inlet and outlet.
  • two compression sleeves are used, which are pushed from both sides onto a clamping tube whose outer diameter increases towards the center. Due to the conical shape of the clamping tube and the conical shape of the inner bore of the pressure sleeves, the pressure sleeves can be pushed onto the clamping tube, with accurate production of the parts, a contact between the inner wall of the pressure sleeve and the outer wall of the clamping tube is done not only punctually, but over the length and cross section of the tensioning tube. Now, if the pressure sleeves pushed with more force on the clamping tube, so the radial pressure of the inner wall of the reinforced
  • the compression sleeves have an outer flange.
  • a screwing device is applied, via which the sliding of the pressure sleeves is regulated on the tension tube.
  • the screw device consists of two screw parts, one of which has an internal thread and an external thread, which can be screwed together.
  • the screw parts are annular and can be pushed from both sides over the pressure sleeve or the pressure sleeves until they hit a fixation.
  • This fixation is typically a mechanical barrier in the form of a flange on the pressure sleeve, or a collar or ring inserted into a groove of the pressure sleeve, typically as
  • Screw member is placed over the free end of the clamping tube and is so narrowed at one end that it can not be pushed completely over the clamping tube but is fixed at the end.
  • the length of the screw is so to the length of the pressure sleeve and the distance between the flange of the pressure sleeve and the end of the clamping tube adjusted so that the voltage applied to the flange screw can be screwed with the voltage applied to the end of the clamping tube screw.
  • the further the two screw parts are screwed, the further the pressure sleeve is pulled onto the tension tube and the stronger the radial pressure of the pressure sleeve on the tension tube.
  • the screw device consists of two screw parts, one of which is an internal thread and a
  • External thread has that can be screwed together.
  • the screw parts are ring-shaped and can be pushed over the pressure sleeves from both sides until they hit the fixation.
  • the length of the screw is adapted to the distance between the fixings on the two pressure sleeves, that the two screw can be screwed together.
  • the screwing can also consist of other means by which the pressure sleeves can be further pressed onto the clamping tube.
  • the screwing can also consist of other means by which the pressure sleeves can be further pressed onto the clamping tube.
  • FIG. 1 shows a preferred embodiment of the holder incorporating chromatographic column.
  • Chromatography column (5) is inserted into the clamping tube (1).
  • the Inner diameter of the clamping tube (1) is chosen so that the chromatography column (5) can be inserted accurately.
  • the outer diameter of the tensioning tube (1) increases towards the middle.
  • two pressure sleeves (2) are pushed.
  • the pressure sleeves are by two screw (3) and (4), which attack on the groove of the two pressure sleeves towards the center of the clamping tube out
  • Screw (3) has an external thread and screw (4) has an internal thread, so that the two screw parts are screwed together.
  • a Endverschraubung (7) is applied, which is screwed onto the pressure sleeves (2).
  • This end fitting serves for the connection of solvent inlet and outlet.
  • the port consists of a capillary port (6), which is also used in conventional chromatography columns.
  • Perforated disk 10 serves to better distribution of the liquid on the sorbent.
  • Circlip 8 and lock washer 9 are assembly aids.
  • Figure 4 shows a pressure sleeve (2), in Figure 5 the tensioning tube (1), in
  • Figure 6 shows the end fitting (7)
  • Figure 7 shows the internal threaded part (4)
  • Figure 8 shows the externally threaded part (3)
  • Figure 9 shows the capillary connection (6).
  • All components of the holder according to the invention may be made of metal, e.g. Stainless steel or mechanically stable, optionally fiber-reinforced,
  • Plastics such as PEEK (polyether ether ketone), PPS (polypropylene sulfide), POM (polyoxymethylene) or PVDF (polyvinyl fluorides) exist. It is also possible that different parts of the bracket
  • the present invention also provides for the use of the holder according to the invention for the pressure-resistant casing of monolithic chromatography columns and monolithic chromatography columns encased in the holder according to the invention.
  • the present invention is also a separation device consisting of the holder according to the invention and a in the
  • the holder according to the invention is for any type of monolithic
  • a monolithic chromatography column also called monolithic column, consists at least of a monolithic sorbent and a jacket.
  • Monolithic sorbents are known in the art.
  • Monolithic sorbents for chromatography consist of a porous shaped body, for example of silica or organic
  • the porous shaped body has at least through pores. Preference is given to monolithic moldings made of silica or silica-containing materials containing a bimodal pore system with macropores or
  • the macroporous size determines the permeability and respectively the column back pressure.
  • the mesopores serve the
  • the monolithic columns are usually coated with polymers such as PEEK or PPS in order to use them in chromatography can.
  • polymers such as PEEK or PPS
  • monolithic sorbents are not pressure-stable coated. However, they must have a liquid-tight sheath. This can be, for example, a shrink tube made of a solvent-resistant plastic.
  • the sorbents may be coated with a conventional sheath of polymers, such as e.g. Be provided PEEK or PPS.
  • the monolithic sorbents are coated in the holder of the invention with a solvent-resistant sheath of plastics such as PEEK or PPS.
  • the sheath can also
  • the device according to the invention typically has suitable end pieces. These correspond to the end pieces typically used in chromatography columns, which allow the solvent inlet and outlet. They may be attached to the column itself, the tension tube or, preferably, to the compression sleeves, e.g. via an end fitting.
  • the holder of the invention is very stable, easy to use and can be reused. By choosing the inner diameter of the clamping tube, the holder can be adapted to each column diameter. Typical diameter of monolithic
  • Chromatography columns are between 1 mm and 25 mm, preferred diameters are between 1 mm and 10 mm.
  • Silica gel diameter 4.6 mm, bimodal pore system with macropores of approx. 1, 1 ⁇ m and mesopores of 15 nm) is placed in the holder according to the invention as shown in FIG. 3 and at a flow rate of 2 ml / min (ACN / water; 40 v / v). This is a

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

La présente invention concerne un élément de retenue pour sorbants monolithiques, présentant comme particularité qu'une pression radiale peut être exercée sur toute la longueur du sorbant par un tube de serrage conique.
EP13712148.9A 2012-04-14 2013-03-22 Élément de retenue pour sorbants monolithiques Withdrawn EP2836830A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13712148.9A EP2836830A1 (fr) 2012-04-14 2013-03-22 Élément de retenue pour sorbants monolithiques

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP12002630 2012-04-14
PCT/EP2013/000871 WO2013152829A1 (fr) 2012-04-14 2013-03-22 Élément de retenue pour sorbants monolithiques
EP13712148.9A EP2836830A1 (fr) 2012-04-14 2013-03-22 Élément de retenue pour sorbants monolithiques

Publications (1)

Publication Number Publication Date
EP2836830A1 true EP2836830A1 (fr) 2015-02-18

Family

ID=47997348

Family Applications (1)

Application Number Title Priority Date Filing Date
EP13712148.9A Withdrawn EP2836830A1 (fr) 2012-04-14 2013-03-22 Élément de retenue pour sorbants monolithiques

Country Status (4)

Country Link
US (1) US20150068979A1 (fr)
EP (1) EP2836830A1 (fr)
JP (1) JP2015513105A (fr)
WO (1) WO2013152829A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3297757B1 (fr) * 2015-05-22 2020-07-15 Merck Patent GmbH Colonne chromatographique et son utilisation
JP6862445B2 (ja) * 2015-11-25 2021-04-21 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ 金属被覆を有するモノリシックな吸着剤
CN107389834B (zh) * 2017-07-12 2022-11-01 中国地质大学（武汉） 一种可视低压同位素分离色层柱

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WO1994019687A1 (fr) 1993-02-26 1994-09-01 Merck Patent Gmbh Separateur
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JPH09119924A (ja) * 1995-08-01 1997-05-06 Hewlett Packard Co <Hp> クロマトグラフィー用分離カラム
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Also Published As

Publication number Publication date
US20150068979A1 (en) 2015-03-12
JP2015513105A (ja) 2015-04-30
WO2013152829A1 (fr) 2013-10-17

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