JPS6052376B2 - liquid chromatography column - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a liquid chromatography column in which a chromatography tube is filled with a filler, a sample is injected into the tube and separated, and various analyzes are performed.

In this type of analysis method, a developing solution (solvent) is added to an ion exchanger, adsorbent, or other packing material, and the mixture is stirred and mixed into a chromatography tube to precipitate the sample. Adsorption and development is carried out by moving the sample and separating it, either directly cutting it out or letting it flow down from the bottom of the chromato tube. Conventionally, after injecting the sample as described above, a load is attached to the top of the chromato tube and development is carried out. Since the liquid was dropped into the chromatography tube and the pressure was used to separate and flow the sample, analysis took time. Incidentally, in order to accurately form a sample separation layer, it is better to make the chromatography tube (filler layer) longer, but the conventional dropwise method requires more time.

Recently, attempts have been made to shorten the time by injecting the developing solution at high pressure, but there is still no technology to removably seal the glass chromatography tube without pressure leaks (liquid leaks) under high pressure. Not developed. In addition, research into filling agents has progressed, and products that can be used repeatedly while still being filled in the tube have been developed, but the high-pressure injection method described above is optimal for efficient use, and the industry is currently developing devices for this purpose. is desired. In view of the above, the present invention uses a glass chromatography tube, completely prevents pressure leakage (liquid leakage) even when a liquid (developing liquid) is injected into the tube under high pressure, and opens and closes the upper and lower ends of the chromatograph tube. The purpose of this invention is to provide a liquid chromatography column that can be freely sealed.

In order to achieve the above object, the present invention provides a chromato tube made of pressure-resistant transparent glass and having screw grooves carved on the outer wall surface of the upper and lower ends, and a chromato tube that is tightly fitted into the openings of the upper and lower ends of the chromato tube in a removable manner. The inner lid has a threaded groove on the inner wall surface to be threaded into the threaded groove, and an outer wall is threaded onto the upper and lower ends of the chromatography tube, respectively, and the inner lid and the outer lid move in synchronization with each other. And,
The inner cover and the outer cover are engaged with each other with a gap that allows for slight relative movement in the axial direction, and the inner cover on the upper end side of the chromato tube is provided with a fitting hole directed in the vertical direction. and an injection tube supported so as to be movable in the vertical direction is fitted into the fitting hole, and a pressure introduction path is formed in the fitting hole to communicate the inside of the chromatography tube with the outside, The chromatography tube is characterized in that a discharge hole is formed in the inner lid on the lower end side of the chromatography tube. The drawings show an example of a liquid chromatography column according to the present invention, and the present invention will be described in detail below based on this example.

In the figure, chromato tube 1 is open at the upper and lower ends to form mouths 2 and 3, and is made of cylindrical pressure-resistant transparent glass. The inner wall surfaces of the mouth portions 2 and 3 are tapered outwardly in width. Reference numeral 6 denotes an inner lid that is removably fitted tightly into the opening 2 at the upper end of the chromato tube 1; A narrow diameter portion 7 is provided protruding from the upper surface side.

Reference numeral 8 denotes an outer cover which has a thread groove 9 carved into the inner wall surface to engage with the thread groove 4 of the tube 1, and is screwed onto the upper end of the tube 1. A fitting hole 10 for fitting is provided, the narrow diameter portion 7 is made to protrude from the hole 10, and the protruding portion. An engaging member 11 that engages with the outer cover 8 is attached to the outer cover 8.

This engaging member 11 is provided to engage the outer cover 8 and remove the inner cover 6 at the same time. In the embodiment, as shown in detail in FIG. 2, the engaging member 11 is configured with a reverse screw nut. This engaging member 11 is screwed 13 onto a small diameter protrusion of the inner cover 6 with a slight gap 12 between the outer cover 8 and the outer cover 8. As a result, the inner cover 6 is pressed by the outer cover 8 and tightly fitted into the opening 2, so even if high pressure is supplied to the pipe 1, liquid will not leak from the fitting part. do not have. Further, when the outer cover 8 is rotated in the removal direction, the engagement member 11 acts to rotate in the tightening direction in the opposite direction, so that the engagement member 11 does not loosen and the inner cover 6 and the outer cover 8 and can move relatively in the axial direction within the range of a slight gap 12, so when the outer cover 8 is rotated in the removal direction, first only the outer cover 8 is engaged within the range of the gap. It will move until it comes into contact with the mating member 11. Therefore, the outer cover 8 can be smoothly rotated in the removal direction (in this case, it is difficult to rotate the outer cover unless the gap 12 is provided). The member 11 may be fixed to the inner cover 6 with bolts or the like, or may be attached by other means. In the center of the inner lid 6 is an injection tube 1.
A fitting hole 15 having a slightly larger diameter than 4 is bored in the vertical direction.

Reference numeral 16 denotes a three-way joint screwed onto the protruding upper end of the inner lid 6. A fitting hole 17, which is common to the fitting hole 15, is bored in the center of the three-way joint 16 in the axial direction.

Reference numeral 18 is a joint screwed onto the upper surface of the three-way joint 16. The injection pipe 14 can freely slide in the center of the joint 18, and a fitting hole 19 for tightly fitting is bored in the axial direction. .

Reference numeral 20 denotes a fixing ring screwed onto the upper part of the joint 18, and a fitting hole 21 with a slightly larger diameter than the injection tube 14 is bored in the center upper part of the ring 20.
A tapered hole 22 extending downward from the hole 21 and widening downward is provided below the hole 21 (see FIG. 3).

Reference numeral 23 denotes a wedge-shaped biting ring with a tapered portion 24 that fits into the tapered hole 22, and a fitting hole 25 into which the injection tube 14 is slidably and tightly fitted is bored in the center (see Fig. 4). ), the biting ring 23 is fitted into the tapered hole 22.

Thus, the injection pipe 14 is connected to the rings 21 and 23 and the joint 1.
8. The three-way joint 16 and the fitting hole of the inner lid 6 are penetrated so that the tip 14a reaches the filler 26 in the chromatography tube 1, and in this state, the fixing ring 20 is rotated and the It is tightened and fixed by the wedge action of the insert ring 23.

27 is a cap nut provided above the fixing ring 20;
8 is a joint with a communicating hole 29 bored in the center in the axial direction and screwed to the cap nut 27 at the lower end; 30 is a cap nut screwed to the upper end of the joint 28;
4b is connected to a cap nut 27, and the top end of the cap nut 30 is connected to a tube 31 whose one end is connected to the side of a syringe S for adding a sample. In this case, the tube 31 may be connected directly to the proximal end 14b of the injection tube 14 without using the cap nuts 30, 27, the joint 28, etc., or by other means. The injection tube 14 may also be configured to be fixedly supported so as to be movable in the vertical direction by other means. Reference numeral 32 denotes a joint screwed onto the side wall surface of the three-way joint 16, and a communicating hole 33 in the axial direction is bored in the center of the joint 32. A communication hole 17a is provided to connect the communication holes 33, 1.
7a, the three-way joint 16, the fitting holes 17, 15 of the inner lid 6, and the injection tube 14. A pressure introduction hole 34 is formed to communicate the inside of the Chromal tube 1 with the outside. ing.

In this case, the pressure introduction hole 34 is the fitting hole 17, 15.
It may be formed by providing a separate hole, or it may be formed by carving a vertical groove in the inner wall surface of the fitting holes 17, 15. When configured in this way, The fitting holes 17 and 15 can be formed to have the same diameter as the injection tube 14 so that they can be tightly fitted. Reference numeral 35 denotes a cap nut screwed onto the distal end side of the joint 32, and the cap nut 35 has one end connected to the pump P side and the other end of a tube 36 connected to the cap nut 35.

In this case, the tube 36 has a cap nut 35 and a joint 3.
Alternatively, the three-way joint 16 may be directly connected to communicate with the communication hole 17a without using the three-way joint 16. Reference numeral 37 denotes an inner cover that is removably tightly fitted into the opening 3 at the lower end of the chromatography tube 1, and a narrow diameter portion 38 is provided on the lower surface of the inner cover 37 in a protruding manner.

Reference numeral 39 denotes an outer cover which has a thread groove 40 carved into the inner wall surface to engage with the thread groove 5 of the chromatography tube 1, and which is screwed onto the lower end of the tube 1.
9 is provided with a hole 41 into which the narrow diameter portion 38 of the inner lid 37 fits;
The narrow diameter portion 38 is made to protrude from the hole 41, and the outer cover 3 is attached to the protrusion.
An engaging member 42 made of a reverse screw nut or the like that engages with the outer cover 39 is similar to the case of the upper end engaging member 11.
They are attached by screws 44 or other means with a slight gap 43 between them (see FIG. 5).

As a result, the inner cover 37 is pressed by the outer cover 39 and tightly fitted into the opening 3, so even if liquid (deploying liquid) is supplied into the tube 1 under high pressure, the liquid will flow from the fitting part. It won't leak.
In addition, since the outer cover 39 and the inner cover 37 are designed to be able to move relative to each other in the vertical direction within the range of a slight gap 43, when the outer cover 39 is rotated in the removal direction, first the outer cover Since only the outer cover 39 moves within the range of the gap 43 until it comes into contact with the engaging member 42, the outer cover 39 can be smoothly rotated in the removal direction. A discharge hole 45 is bored in the center of the inner lid 37 in the axial direction, and a fifth hole is formed in the upper surface.
As shown in detail in FIG. 6, an arbitrary number of annular grooves 46 are carved to surround the discharge hole 45, and
is connected to the discharge hole 45 by a radially carved groove 47. 48 is a filter placed on the upper surface of the inner lid 37;
49 is a joint screwed onto the lower end protrusion of the inner lid 37;
A two-way joint 50 is screwed to the bottom of the joint 49,
A nozzle 51 is attached to the lower part of the two-way pot 50.

In the figure, 32 is a pressure gauge installed in the tube 36, 35 is a developing liquid tank, and 54 is a suction pipe connecting the pump P and the liquid tank 53. The injection tube 14 is made of stainless steel or Teflon, and the inner lids 6, 37, outer lids 8,
39. The engaging members 11, 42, three-way joint 16, joint, cap nut, tube, and other components are made of chemically resistant materials that can withstand acids, alkalis, organic solvents, etc.
For example, it is made of Teflon, etc. The present invention has the above structure, and an example of its usage will be explained below.

First, place the filter 48 on the inner cover 37 on the lower side, fit the inner cover 37 to the mouth part 3, and screw the outer cover 39 onto the tube 1. The engaging member 42 is screwed on, and the joint 49 and . The pots 50 are connected and the pots 50 are closed.

In this case, it is also possible to assemble the above-mentioned parts in advance, rotate the outer cover 39, and simultaneously perform the fitting of the inner cover 37 and the screwing of the outer cover 39. This allows chromatography tube 1
The lower end of is completely sealed. Next, a developing solution (solvent) is added to the ion exchange agent, adsorbent, and other fillers 26, and the mixture is stirred and poured into the chromatography tube 1.
Insert the inner lid 6 into the mouth 2 on the upper side in the same manner as described above, screw the outer lid 8, and screw the engaging member 11 and three-way joint 16 onto the upper end of the inner lid 6. A joint 32 and a cap nut 35 are screwed onto the side wall surface of the three-way joint,
In addition, the injection tube 14 is fixed to the joint 18 and the ring 20 at the upper part of the three-way joint 16, and the injection tube is inserted into the fitting holes 17 and 15 so that the tip 14a faces the inside of the chromatography tube 1. The cap nuts 27, 30 and the joint 28 are connected to the proximal end of the injection tube 14, and the tube 1 is supported by a suitable support (not shown) and kept stationary upright. Then, after a certain period of time, the filler 26 is precipitated, and as shown in the first and second figures, a layer of the filler 26 is formed in the tube 1, and a layer of the developing liquid 55 is formed on the upper part, and the injection tube 14 is The tip 14a of is located near the top of the filler 26.
In this case, if the tip 14a of the injection tube 14 does not reach into the filler 26, the sample will be injected into the developing solution 55 and diluted, which is not preferable in terms of efficiency. Therefore, the injection tube 14 is adjusted with the ring 20 so that its tip 14a reaches the filler 26 to determine its fixed position. Further, the injection tube 14 and other parts may be attached after the filler is precipitated. Therefore, after injecting a predetermined amount of the sample in the cylinder S from the tip 14a of the injection tube 14, the pump P is driven to remove the developing liquid 55 in the liquid tank 53.
When a is supplied under pressure, this developing liquid 55a is introduced into the tube 1 through the pressure introduction path 34.

Therefore, the sample 56 in the tube 1 rapidly expands and moves, and as shown by the chain line in FIG. Ru. So the bottom part! When the two-way pot 50 is opened, the samples A, B, and C separated as mentioned above flow down sequentially from the discharge hole 45 through the filter 48, and are detected by a detector or the like. In addition, in the embodiment, a discharge hole 45 is provided on the top surface of the inner lid 37.
An annular groove 46 surrounding the S groove 46 and a radial groove 47 connecting the S groove 46 and the discharge hole 45 are provided in a spider web shape, so that the sample remains separated in the tube 1 (in the capillary tube). Since the contact cross-sectional area of the two liquids is small, the two liquids do not mix or move back and forth, but instead flow in the order of the two liquids (first and second) in the order of A → developing liquid → B. → Developing solution → It can be separated and drained as shown in C.
When the sample 56 in the tube 1 flows out of the tube 1, the lower pot 50 is closed, the sample is supplied into the tube 1 in the same manner as above, and then the developing solution is supplied, and this pattern is repeated. This enables continuous analysis, etc.

Next, when removing the cap from the chromato tube, use the outer lid 8.
, 39, the inner lids 6, 37 are also pulled and pulled out at the same time.

As described above, the present invention comprises a chromato tube made of pressure-resistant transparent glass and having screw grooves carved on the outer wall surface of the upper and lower ends, an inner lid that is removably fitted tightly into the openings of the upper and lower ends of the chromato tube, respectively; The inner wall surface has a thread groove that engages with the thread groove, and the chromato tube has an outer cover that is screwed onto the upper and lower ends of the chromato tube, respectively, and the inner cover and the outer cover at the upper and lower ends of the chromato tube are synchronized, respectively. The inner cover and the outer cover are engaged with each other with the problem of being able to move relative to each other in the axial direction. A fitting hole is bored, and an injection tube supported so as to be movable in the vertical direction is fitted into the fitting hole, and a pressure introduction path is provided in the fitting hole to communicate the inside of the chromatography tube with the outside. is formed, and a discharge hole is formed in the inner lid on the lower end side of the chromato tube.According to the present invention, the following effects are achieved.

(a) The inner lids that are tightly fitted to the openings at the upper and lower ends of the chromato tube are engaged with the inner lids and are held down by the outer lids that are screwed onto the upper and lower ends of the chromato tube. It can be completely sealed and completely prevent liquid leakage even if high pressure (hydraulic pressure) is introduced into the chromato tube.

(b) The upper and lower inner and outer lids are designed to be able to move relative to each other in the axial direction within a certain gap, so when rotating the outer lid in the removal direction, first only will move within the gap.

Therefore, the outer cover can be smoothly and easily rotated toward the removal side (in this case, if a gap is not provided, the outer cover will be rotated while also moving the inner cover from the beginning,
(The outer lid is difficult to rotate.) (C) Since the upper and lower inner and outer lids are engaged so as to move in synchrony, the inner lid can be easily and smoothly removed.

(d) Since the injection tube is supported so as to be movable in the vertical direction, the position of the tip of the injection tube can be adjusted to a position suitable for injection of the sample, so that the injection of the supple can be carried out well.

(e) Since the fitting hole formed in the inner cover at the upper end of the chromato tube has a pressure introduction hole that communicates the inside of the chromato tube with the outside, the pressure (developing liquid) is applied to the filler layer inside the chromato tube. Therefore, even if the sample gets mixed into the developing liquid layer formed above the packing material (when the sample is injected, some of it may float above the packing material). ), it can be pressed downward to quickly and efficiently develop and move and separate.

[Brief explanation of drawings]

The drawings show an embodiment of the liquid chromatography column according to the present invention, and FIG. 1 is a longitudinal sectional view, FIG. Fig. 4 is a longitudinal sectional view of the ring, Fig. 4 is a longitudinal sectional view of the biting ring, Fig. 5 is an enlarged longitudinal sectional view of the sealing part on the lower side, and Fig. 6 is a bottom view of the inner lid on the lower side. . 1... Chromatography tube, 2, 3... Mouth part,
4, 5... Thread groove, 6, 37... Inner cover,
8, 39... Outer lid, 9, 40... Screw groove, 11, 42... Engaging member, 13...
・Screwing, 14...Injection pipe, 15...Fitting hole, 16...Three-way joint, 17...Fitting hole, 17"a... ...Communication hole, 18...Joint, 20...Fixing ring, 23...
... Biting ring, 26... Filler, 31, 36...
...Tube, 33...Communication hole, 34...
...Pressure introduction path, 53 ...Liquid tank, 55, 55
a...Developing solution, 56...Sample, P
...Pop, S...Syringe.

Claims (1)

[Claims] 1 (a) A chromato tube made of pressure-resistant transparent glass and having screw grooves carved into the outer wall surface of the upper and lower ends; (b) Inner lids that are removably fitted tightly into the openings of the upper and lower ends of the chromato tube, respectively; (c) an outer lid having a threaded groove on the inner wall surface that engages with the threaded groove, and screwed onto the upper and lower ends of the chromato tube, respectively; (d) an inner lid on the upper end side of the chromato tube facing vertically (e) an injection tube that is fitted into a fitting hole drilled in the chromatotube, and whose tip is positioned above the filling material filled in the chromatotube; and a pressure introduction path that airtightly communicates the upper end of the chromatography tube with the outside via a The inner cover and the outer cover are moved in synchronization with each other, and the inner cover and the outer cover are held relatively independently within the range of the gap with respect to the axial direction. The injection tube is engaged with each of the inner lids so as to be movable in the vertical direction, and the injection tube is movable in the vertical direction.
The proximal end side of the chromato tube is kept airtight with the inside of the chromato tube, and its base end side is supported by a support member provided on the upper part of the inner lid on the upper end side of the chromato tube, and the inner lid on the lower end side of the chromato tube is A discharge hole is formed, and after a sample is injected into the filling material of the chromato tube through the injection tube, a developing solution is supplied under pressure to the upper end of the chromato tube through the pressure introduction path. . A liquid chromatography column, characterized in that the sample is developed and moved within the packing material layer to be separated.