JPH01199156A - Adjustable distribution chamber apparatus - Google Patents

Abstract

PURPOSE: To positively perform close sealing at a column window part by providing a seal adjusting pipe with first and second sealing elements that can be operated independently for forming a liquid-tight sealing between a distribution chamber and a column pipe. CONSTITUTION: A first seal 70 is compressed so that a liquid-tightly engaged state can be achieved with the inner wall of a column pipe 10 by clamping each of a seal adjusting lever 10. When a traveling phase medium is supplied to a column via a distribution chamber 100 with a desired usage power, the traveling phase medium that is not compressed dyer passes a second seal 90 and flows into the seal 70 along a seal adjusting bath 50. Then, the seal adjusting lever 120 is clamped and the second seal 90 is compressed, thus forming a liquid-tight seal between an operation column layer and the upper edge of the distribution chamber 100, thus preventing the traveling phase medium in used pressure being captured between the seals 70 and 90 from being leaked outside the observation window 40 over the two seals of the seal 90 even if the seal 70 becomes defective.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to an adjustable distribution chamber device for a chromatography column, and more particularly to an adjustable distribution chamber device for a chromatography column, and more particularly to the distribution of small amounts of mobile phase medium ( The present invention also relates to a chromatography column using the distribution chamber device of the present invention.

[Conventional technology]

The use of column chromatography to separate chemicals is well known. Separation of chemical species occurs through the interaction of sample, stationary phase, and mobile phase. The stationary phase is a dispersed medium with a large surface area through which the mobile phase can flow. The chemistry of the stationary phase provides significant control over the separation process. The greater the affinity of a particular compound (solute) for the stationary phase medium, the longer that substance will be retained in the stationary phase. Various attractive forces such as van der Waals forces, hydrogen bonds, ionic bonds, and complex formation in reversible reactions such as antigen-antibody reactions act as retention forces.

Chromatography columns are constructed from a relatively small number of parts. Cylindrical columns filled with stationary phase media are joined by a bottom chamber that allows the mobile phase media to pass through but not the stationary phase. The top or "dispensing" chamber directs the sample and mobile phase medium above the stationary phase medium. Many columns have the same bottom chamber and distribution chamber (in which case both are referred to as "terminal chambers"), such that the column can be used in either direction. It is necessary to install a seal to prevent the mobile phase medium and sample from leaking from the terminal chamber to the outside of the column.

During column chromatography operations, the mobile phase permeates through the column either by gravity or under pressure.

High pressure stainless steel industrial column is 2ooK9/a
d (3000 pai), but acrylic, glass, and standard stainless steel-clad columns typically use up to 1. o a 3Kgt/cdcls psi) to 4.1a zKgf/nl, 3,099Kgt
/ca.

It is used within the range of 6.714Kgr/ctA.

Although the selection of stationary and mobile phase media is extremely important, it will not be discussed here. Separation of bimolecular entities based on size rather than charge is often achieved using porous gels, and silica is generally the stationary phase medium of choice. Commonly used mobile phase media include nonpolar true chain hydrocarbons, aromatic hydrocarbons, and ethers, as well as ethers of intermediate polarity, and highly polar alcohols and water.

[Problem that the invention seeks to solve]

Column chromatography in the laboratory has long been carried out in glass biurets containing handmade stationary phases, but adapting column chromatography to large-scale industrial separation processes requires chromatography. Graphic technology F
6 For example, it is known that accurate separation of a sample requires uniform distribution of the sample across a column of stationary phase media. The upper sample needs to be dispensed directly onto the medium, ie with a minimum of head space between the dispensing chamber into which the sample is fed and the top of the medium. Since the height of the media-filled column section can vary depending on the compound product to be separated for each use or due to expansion and settling of the stationary phase media immediately after media loading, an adjustable distribution chamber is used. The device was well received in industry.

U.S. Pat. No. 3,487,938 is directed to an automatic headspace reduction device and provides a mobile piston that rests on top of a column of chromatographic media. The piston automatically moves according to the position of the top of the column to minimize headspace when the media layer expands and contracts.

US Pat. No. 3,483,986 (A.G. Wright) relates to a column chromatography device. An adjustable terminal chamber device useful for distributing mobile phase media and sample across the top of the stationary phase media layer of a column is disclosed in that patent.

Published European Patent Application No. 8.921 (A.G. Wright) also discloses an adjustable terminal chamber arrangement for a chromatography column.

[Means for solving problems]

The aforementioned cyclocolumns can be made of acrylic, glass or stainless steel. Adjustment of the height of the distribution chamber is easily accomplished in transparent acrylic or vitreous columns where the top of the media layer of the column and the bottom of the distribution chamber are visible. but,
Adjustment of the distribution chamber in stainless steel columns is difficult because neither the distribution chamber nor the top of the media packed bed are visible inside the column.To eliminate this drawback of otherwise desirable stainless steel columns, the present invention was developed. One aspect of the invention provides a stainless steel column containing a plurality of viewing windows. This viewing window is positioned so that the person operating the column can see the top of the stationary phase media and correctly position the distribution chamber at the top of the stationary phase media bed.

Another aspect of the invention is a chromatography column,
BRIEF SUMMARY OF THE INVENTION The apparatus of the present invention provides an improved adjustable distribution chamber system particularly for use in windowed columns. A seal conditioning tube having first and second sealing elements is provided. A band of mobile phase medium, preferably at the working pressure of the column, is allowed to form between the first and second seals, ensuring a tight seal at the column window.

〔Example〕

FIG. 1 shows a chromatographic apparatus including a column tube 10 standing on a bottom 20, the layer of stationary phase medium contained in the column tube is not shown, and the column tube 10 has flanges 15 and 5 at each end. 6, the adjustable distribution chamber device 30 according to the invention is attached to the upper flange 15 and partially located inside the column tube 10. As shown in FIG. 1, the distribution chamber device 30 is attached to the column tube flange 15 by a plurality of height adjustment rods 35. As shown in FIG.

The illustrated embodiment is a stainless steel column containing a plurality of windows 40, the structure and function of which will be described below.

FIG. 2 shows a more detailed view of the adjustable distribution chamber device 30.As shown in FIG. Configure. Seal conditioning tube 50 contains two independently actuatable seals comprised of compressible O-rings in this preferred embodiment. The first seal 70 is located in the left groove formed between the upper shoulder of the seal adjustment tube 50 and the seal adjustment ring 80. A second seal 90 is placed in a similar groove between the lower layer of seal conditioning tube 50 and distribution tube 100. The first seal 70 and the second seal 90 each have one set of seal adjustment rods 110.
and 120 (ie, compression and release are performed). For clarity, only one of each set of adjustment rods 110 and 120 is shown in FIG. The details of the operation of this device will be described later, but by turning the seal adjustment rod in one direction, the seal adjustment ring 80 is pressed downward against the seal adjustment tube 50, so that the first seal is compressed. Suffice it to say, the second seal 90 is located on the seal adjustment rod 1.
Similarly, the distribution chamber ioo is compressed by turning 20 to force the distribution chamber ioo upwardly into the seal adjustment tube 50.

The distribution chamber Zoo is fluidly connected to a source of mobile phase medium, as shown in FIG. 5, and serves to uniformly distribute the mobile phase medium across the top of the stationary phase medium packed bed. This preferred distribution chamber is the distribution chamber 100
A colored porous sintered screen 102 is provided above a plurality of channels 104 formed on the surface of the screen. The mobile phase medium flows along the flow path through the sintered screen and onto the stationary phase medium layer as indicated by the arrows in FIG.

Figures 3A and 3B illustrate the adjustable distribution chamber apparatus of the present invention in further detail. As shown in FIG. 3A, seal adjustment rod 110 serves to adjust the first seal 70, which in this preferred embodiment is a compressible elastomer o-ring. and the corresponding chamfered shoulder 82 of the seal adjustment ring 80 . O
- the ring 70 is not compressed in FIG. 3A and the column tube l
It is shown barely touching the inner wall of the O. Compression of the O-ring is achieved by turning the seal adjustment rod clockwise, 9 degrees, to move the threaded end 112 of the seal adjustment rod 110 over the corresponding threaded end of the stud 130 until the seal spring 54 is compressed. This acts to bring the seal adjustment ring 80 and seal adjustment tube 50 closer together against the force of. 0-
When the ring is compressed, it forms a virtually liquid-tight seal against the inner wall of the column tube IO. The seal 70 is returned to its original position by turning the seal adjustment rod 110 counterclockwise.The end 112 of the seal adjustment rod 110 moves upwardly along the stud 130 while the spring 54 moves the seal adjustment tube 50 and the seal adjustment ring 80. It acts to keep away from.

As shown in FIG. 3A, the seal adjustment tube 50 is connected to the conduit 145.
a conduit 145 including an orifice 140 in fluid communication with
is configured to contain a pressure sensor (not shown) that senses the pressure of the mobile phase medium trapped between seals 70 and 90 during column operation. If a pressure sensor is not used, orifice 14
G should be covered with orange.

The mechanism for adjusting the second seal 90 is shown in Figure 3B. Similar to the first seal 70, the second seal 90 is
Shoulder 56 of seal adjustment tube 50 and chamfered shoulder 1 of distribution chamber 100
02.

The second seal 90 is compressed by turning the seal adjustment rod 12G clockwise, causing the threaded end of the implantable port 130 and the distribution chamber Zoo to press against the action of the spring 54 into the seal adjustment tube 50. being pulled upwards. Therefore, the adjustment mechanism of the first seal and the adjustment mechanism of the second seal are virtually the same.

FIG. 4 shows an adjustable distribution chamber device 30 mounted within the upper end of a chromatography column tube 10, the column tube 10 having a plurality of viewing windows 40, only one of which Illustrated.

As seen in FIG. 4, the window 40 includes a plate 42 of glass or other transparent material mounted inside a correspondingly shaped opening in the column tube. A layer of packing material 44 is applied between the window plate 42 and the wall of the column tube 10, and a cover plate is secured to the empty inlet tube.

Next, the operation will be explained. Chromatographic separation is performed by first preparing a packed bed of stationary phase medium with its top positioned between the top and bottom of the window 40.
Implemented within the columns of Figures and Figure 4. Means for preparing packed beds are well known. Lower the adjustable distribution chamber device 30 into the column tube IO, making sure that the height adjustment rod 35 fits into the corresponding hole in the column flange 15. Lower the distribution chamber apparatus 30 to a position where the distribution chamber 100 is about to touch the top of the packed bed, and then tighten the height adjustment nut 36 to secure the distribution equipment R30 in place. Each of the seal adjustment rods 110 is tightened to compress the first seal 70 into fluid-tight engagement with the inner wall of the column tube IO.

Once the mobile phase medium is fed to the column through the distribution chamber 100 at the desired working pressure, the mobile phase medium (not yet compressed) passes through the second seal 90 and along the seal conditioning tube to the first seal 70. It flows into the area. The seal adjustment rod 120 is then tightened to compress the second seal and form a liquid-tight seal between the working column layer and the top of the distribution chamber. A pressure sensor mounted inside conduit 145 is used to verify that the pressure of the mobile phase medium trapped between seal 70 and seal 60 is virtually the same as the pressure of the mobile phase medium in the column. can be used for first seal 7
Even if there were any blemishes in the integrity of the first seal 90, the mobile phase medium at the working pressure trapped between the first and second seals and ultimately the second seal 90 Helps prevent leakage beyond the seal and out of the column.

The specific examples of the invention shown and described herein are for purposes of illustration only. Various structural and operational modifications will occur to those skilled in the art. For example, the adjustable distribution chamber device of the present invention is well suited for use with windowless chromatography columns and can be operated with only one of the two compressible seals compressed. . It is intended that such modifications be considered a part of the present invention insofar as they come within the spirit and scope of the appended claims.

[Brief explanation of the drawing]

FIG. 1 is a drawing of a chromatography column and an adjustable distribution chamber according to the invention; FIG. 2 is a perspective view with a portion of the adjustable distribution chamber of FIG. 1 in cross-section; FIG. Figure 3B is a cross-sectional view of the adjustable distribution chamber taken along lines A-A and B-B in Figure 2, respectively. Figure 4 is a cross-sectional view of the adjustable distribution chamber shown in Figure 2 with a window installed in the chromatography column. FIG. 5 is a plan view with a portion of the adjustable distribution chamber in cross-section; FIG. 5 is a cross-sectional view of a preferred distribution chamber of the apparatus of the invention; B/Qi, 3s Drawing 1; 1・1゛; FIG, 5 Procedural amendment (method) (Examiner) 1. Indication of the case 1985 Patent Application No. 1611+10 2
Name of invention-99, distribution room device 3 that can adjust the classification of designated products, relationship with the amended person case Patent applicant 4, agent

Claims (1)

[Claims] 1. An adjustable distribution chamber device for a chromatography column including a column tube, a stationary phase medium layer, and a mobile phase medium, for installing the distribution chamber device on the top of the column tube. a support means including means for adjusting the height of the distribution chamber arrangement within the tube; and a second seal-forming element configured to engage the inner wall of the column tube with the sealing means depending from the support means. a seal configured to engage an inner wall of the column tube with the adjustable sealing means and the sealing means disposed between the second adjustable sealing means and the support means and depending from the support means; first adjustable sealing means comprising a forming element, each said adjustable sealing means having a first position in which said seal-forming element is not in liquid-tight engagement with the inner column wall; An adjustable dispensing chamber device characterized in that the adjustable dispensing chamber device is independently adjustable between a second position in liquid-tight engagement with the second position. 2. A patent in which the first and second sealing means each include a compressible seal-forming element which, when compressed, engages the inner wall of the column in a liquid-tight manner. Apparatus according to claim 1. 3. The first and second sealing means sometimes include a seal adjustment tube suspended from the support means by a plurality of seal adjustment rods, and the first set of the seal adjustment rods is connected to the first seal adjustment tube. 2. Apparatus according to claim 1, wherein said seal adjustment rods of said second set are arranged to adjust said second adjustment means. 4. The apparatus of claim 1, wherein said seal regulating tube includes means for receiving pressure sensing means. 5. The apparatus of claim 1 further comprising flow distribution means for distributing the mobile phase medium to the stationary phase medium layer. 6. The device of claim 2, wherein said seal-forming element comprises an o-ring. 7. Adjustable distribution chamber device according to claim 1 in combination with a chromatography column tube. 8. The apparatus of claim 7, wherein the chromatography column tube is provided with a window disposed in its side wall. 9. preparing a column tube, inserting an adjustable distribution chamber device into the column tube, adjusting a first adjustable sealing device to provide a virtually liquid-tight seal, and preparing a mobile phase; A method of performing column chromatography comprising the steps of supplying a medium at a working pressure to the column and adjusting a second adjustable sealing means to provide a substantially liquid-tight seal.