JP2587162Y2 - Liquid chromatograph mixer - Google Patents

Description

[Detailed description of the invention]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a mixer for a liquid chromatograph capable of obtaining a sufficient mixing effect with a small volume.

[0002]

2. Description of the Related Art In a gradient analysis using a liquid chromatograph, for example, as in Japanese Utility Model Application Laid-Open No. 3-76163, a plurality of eluents are uniformly mixed by inserting a mixer between a liquid sending pump and a sample injector. Mixed.

Heretofore, this type of mixer has filled a large number of spherical glass beads into a straight tubular mixing pipe or a mixing block, introduced an eluent between the glass beads, and made the meandering and turbulent flow. To get the desired effect.

[0004]

However, this conventional mixer generally has poor mixing efficiency, and takes a long time from the start of mixing until a predetermined solute concentration is obtained, resulting in poor responsiveness and the mixing required for this. There is a problem that the volume becomes large, and the diameter and length of the mixing pipe become long, and the size of the mixing block becomes large.

The present invention solves such a problem, and a sufficient mixing effect can be obtained with a small volume, the responsiveness can be improved, and at the same time, the mixer is easy to manufacture , the size and weight of this type of mixer can be reduced, and the space for installing a column can be reduced. It is an object of the present invention to provide a liquid chromatograph mixer capable of achieving the following.

[0006]

For this reason, the liquid chromatograph mixer of the present invention is interposed between a column for mixing a plurality of eluents and a column and wound in a coil shape.
In a liquid chromatograph mixer in which a number of spherical mixing members are filled inside a mixing pipe , a straight tube is used.
Many spherical mixing members inside the mixing pipe
Provide a mixer that is filled several times and formed into a coil shape.
Place the column inside the sir and mold it into a coil
Filling a mixing member in a mixing pipe
Compared to this, it can be filled quickly and densely,
To improve the mixing effect
Column by utilizing the dead space of the
The installation space can be reduced.

[0007]

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 to FIG. 3 show an embodiment of the present invention in which a high pressure gradient analysis is performed using a preparative column having an inner diameter of about 20 mm. And eluents 3 and 4 which are different from each other are accommodated in the conduits 5 and 6, respectively.
Is inserted.

The liquid feed pumps 7 and 8 can be controlled in drive timing and flow rate setting via a controller mounted on the liquid chromatograph or a separate microcomputer (not shown). 4 can be sequentially prepared.

The downstream side of the conduits 5 and 6 communicates with a mixer 10 installed in an oven 9, and the sample injector 1 is connected to a conduit 11 piped to the outlet side of the mixer 10.
2 is connected, and the fractionation column 13 is connected to the downstream side.

As shown in FIG. 2, the mixer 10 is formed by winding a mixing pipe 10a having a corrosion resistance such as a stainless steel tube and a predetermined mechanical strength into a coil shape, and the inner diameter thereof is used under the same analysis conditions. It is configured to be approximately 1/5 of the conventional product, approximately 4 mm in the embodiment, and the length is approximately 5 mm of the conventional product.
The length is about 10 to 10 times, and approximately 5 m in the embodiment.

Therefore, the volume in the mixing pipe 10a, that is, the value obtained by multiplying the cross-sectional area in the pipe by the length of the pipe corresponds to approximately 1/5 to 1/2 of the conventional product used under the same analysis conditions.

The inside of the mixing pipe 10a is tightly filled with a spherical mixing member 14 such as a stainless steel ball, a Teflon-based synthetic resin ball, so-called PTFE ball, glass beads, or the like.
The eluent has an outer diameter of about 1 mm, which is substantially the same diameter as a conventional product used under the same analysis conditions, and moves the eluent through the gap between the members 14 and the inner surface of the mixing pipe 10a. Let me. Therefore, the mixing member 14
The ratio of the inner diameter of the mixing pipe 10a to the outer diameter of the conventional pipe is about 1/20, while that of the conventional pipe is about 1/20 in the present invention.
/ 5 to 1/2.

A column 13 is provided inside the mixer 10 as shown in FIG. 2, and a detector 15 for detecting a predetermined solute and measuring its concentration is connected downstream of the column 13.
A waste liquid reservoir 16 is provided at the downstream end.

In the figure, reference numerals 17 and 18 denote mixing pipes 10.
The joints 19 and 20 are connected to the outside of the nut attached to the end of the pipe a.

[0015]

In order to manufacture the liquid chromatograph mixer having the above-described structure, for example, a straight tubular mixing pipe 10a having a predetermined inner diameter and length is prepared, and a fine mesh filter (not shown) is provided at one end thereof. The mixing member 14 having a predetermined size is placed in the pipe from the other end and filled.

In this case, the mixing pipe 10a has a length of about 5 to 10 in comparison with a conventional mixing pipe used under the same analysis conditions, instead of reducing the inner diameter to about 1/5.
The length is doubled, and the pipe length is made shorter for the above-mentioned smaller diameter.

That is, in order to obtain the same mixing capacity as the conventional one with the above-mentioned pipe diameter, the mixing pipe 10a
The length should be approximately 25 times as long as the conventional length, but is set to approximately 5 to 10 times as long as 1/5 to 1/2 of the calculated value. In other words, it means that the volume of the mixing pipe 10a is approximately 1/5 to 1/2 of the conventional volume.

In the above filling, since the mixing pipe 10a is a straight tube, the member 14 is filled quickly and densely as compared with the method of filling the mixing member 14 after winding it into a coil shape. You.

Next, similar filters (not shown) are arranged at the other end of the mixing pipe 10a, and joints 19 and 20 are screwed from outside the filters to plug the pipe ends. The mixing pipe 10a may be wound into a coil having a predetermined diameter via the device and the device.

In this case, the relatively long mixing pipe 10a is formed to be short when the pipe is straight, so that even when the mixing pipe 10a is arranged in the column oven 9, its installation space is compact, and the column oven 9a is compact. Promote miniaturization of itself. Further, at the time of the above-mentioned winding, the bending pressure of the mixing pipe 10a acts on the mixing member 14, but since the member 14 is spherical, it freely moves according to the pressure and escapes from the pressure action, so that it is crushed. Absent.

When the mixer 10 manufactured as described above is placed in the column oven 9, the mixer 10 is reduced in size as described above, and the column 13 is inserted and placed in a so-called dead space inside the mixer 10. As a result, the installation space for the column 13 is saved, and the size of the column oven 9 is further reduced. In particular, this advantage has a great effect under conditions where the size of the column is increased and the size of the mixer 10 is accordingly increased as in preparative chromatography as in the examples.

Next, when the gradient analysis is started using the mixer 10, the respective eluents 3 and 4 are adjusted to a predetermined composition through the respective liquid sending pumps 7 and 8, and the mixed solution is transferred to the downstream side. It is sent out and guided to the mixer 10 in the column oven 9.

The mixed solution moves in a meandering and turbulent flow repeatedly between the mixing members 14 filled in the mixing pipe 10a and the gap between the mixing member 14 and the inner surface of the mixing pipe 10a. Mixing is uniform.

In this case, since the mixing pipe 10a is formed in a curved tubular shape, the eluent constantly changes its moving direction, and the above-mentioned meandering and turbulent flow are promoted, so that the moving distance can be relatively enlarged. Then, it goes around the mixing member 14 and the peripheral surface of the pipe 10a facing the flow path and comes into close contact with them.

When this is compared with the conventional mixing, the conventional eluent moves in the tube in a generally straight line and the direction thereof is uniform, so that the frequency of the meandering and turbulent flow is small, and
Moreover, since there is a dislike for contact with the specific peripheral surface of the mixing member, the mixing effect is generally poor.

That is, the present invention relates to the mixing pipe 10
Although the volume of “a” is smaller than the conventional one, a precise and high-quality mixing effect can be obtained, and a gradient analysis with good reproducibility can be performed. The time from the start of mixing to the detection of a solute component at a predetermined concentration can be shortened, and the responsiveness of this kind of analysis can be improved.

For example, when performing a gradient analysis using a preparative column having an inner diameter of about 20 mm as in the embodiment, the flow rate is 10 to 20 mL / min. Therefore, a conventional mixer requires a capacity of 20 to 40 mL. According to the present invention, even in this case, a gradient fraction collection with sufficient reproducibility can be performed with a volume of about 10 mL.

FIG. 4 shows a chromatogram obtained under the same analytical conditions using the present invention and a conventional mixer configured to a volume of 10 mL. That is, according to this experiment, the product according to the present invention shown in FIG. 7A has a very high peak value as a whole compared with the conventional product shown in FIG. Therefore, it was confirmed that a high-concentration solute component could be detected quickly.

As described above, the mixer 10 of the present invention has a simple structure, but can obtain a sufficient mixing effect with a small volume, and can reduce the size of the mixer and improve the responsiveness of analysis. If installed inside
The size of the oven 9 can be reduced.

[0030]

[Effects of the Invention] The liquid chromatograph mixer of the present invention has a spherical mixing mixer inside a straight mixing pipe.
A mixer that is filled with a large number of
Because of the radiation, the mixing pipe
Quicker and more precise than those that fill the mixing member
Can be filled and easily manufactured, and mixin
Can improve the effect. Also inside the mixer
The dead space of the mixer
Utilize and arrange columns, saving column installation space
There is an effect that can be achieved .

[Brief description of the drawings]

FIG. 1 is an explanatory view showing an embodiment of the present invention.

FIG. 2 is an enlarged front view showing a main part of one embodiment of the present invention.

FIG. 3 is an enlarged partial cross-sectional view showing a part of the present invention.

FIGS. 4A and 4B show chromatograms obtained by using the mixer of the present invention in comparison with a conventional example. FIG. 4A shows a case where the mixer according to the present invention is used, and FIG. It shows the case where it is done.

[Explanation of symbols]

 3, 4 Eluent 10 Mixer 10a Mixing pipe 14 Mixing member

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. ⁶ , DB name) G01N 30/34

Claims (1)

(57) [Scope of request for utility model registration] 1. A column and a column for mixing a plurality of eluents.
Mixing pipe inserted between and wound into a coil
In a liquid chromatograph mixer in which a number of spherical mixing members are filled, a straight tubular mixing
Fill the inside of the pipe with a number of spherical mixing
And a mixer shaped like a
A liquid chromatograph mixer comprising the column .