JP2603770Y2 - Gradient mixer for liquid chromatography - Google Patents

Description

[Detailed description of the invention]

[0001]

Industrial Applicability The present invention makes it possible to change the mixing capacity of a mixer with a simple structure, easily and precisely change the composition of a solvent, and freely set the analysis time, the retention time of each peak component, or the time for solvent replacement. The present invention relates to a gradient mixer for a liquid chromatograph, which can be improved to improve the non-separation of components.

[0002]

2. Description of the Related Art In gradient analysis by liquid chromatography, generally different solvents are sent to a mixer and then sent to a column while sequentially changing the solvent composition.

However, since the mixing volume of the conventional mixer is constant, when a desired solvent composition is obtained at a certain time,
The operation has to be changed to a mixer having a different capacity, gradient conditions, or solvent composition, which makes the operation complicated and troublesome.

[0004]

SUMMARY OF THE INVENTION The present invention solves such a problem, and the mixing capacity of the mixer can be easily and precisely changed with a simple configuration, and the analysis time, the retention time of each peak component, or the solvent replacement. The time can be changed arbitrarily, the separation of components is improved , and the cross-sectional shape of the mixing chamber
Promotes diversification, improves mixing efficiency, and
Prevents rotation and twist of conduit connected to plunger with simple configuration
It is another object of the present invention to provide a gradient mixer for a liquid chromatograph in which the piping can be easily and compactly formed .

[0005]

Means for Solving the Problems] Therefore, the liquid chromatograph gradient mixer of the present invention comprises a body having a mixing chamber inside, fitted to be movable in the mixing chamber, and
Plunger in which a guide hole communicating with the mixing chamber is formed.
Between the plunger and the rotation
Adjustment that allows the plunger to move axially through the position
A knob and one end connected so as to be able to move with the plunger
Said guide holes and a conduit communicating with, the gradient mixer for liquid chromatograph adjustable volume of the mixing chamber through the displacement of the plunger, the flop
Adjusting the cylinder that slidably supports the runner
And the cylinder can be displaced to the body.
Screwed onto the end of the plunger
The locking piece is adjusted with the end of the cylinder.
The plunger is engagable with the inner end of the plunger.
Can be moved linearly in the axial direction, the mixing capacity of the mixer can be easily and precisely changed with a simple configuration, and the analysis time, the retention time of each peak component, or the time for solvent replacement can be arbitrarily changed, improve nondisjunction components, yet mixed
Encourage diversification of cross-sectional shapes of joint rooms to improve mixing efficiency
And a simple configuration for connecting the conduit to the plunger.
Prevents rotation and torsion, making the piping easy and compact
Is the feature that it has to so perform.

[0006]

[ Operation ] Operate the adjustment knob to move the plunger to the mixing chamber.
Move and make the volume of the mixing chamber variable with a simple configuration. The mixing capacity of the mixer is variable, and the composition of the solvent can be easily and precisely adjusted , and the analysis time and each peak component can be retained.
Time or solvent replacement time can be changed arbitrarily, and
Improve the separation of components . Slidably supports plunger
When the cylinder to be held is provided so as to be movable with the adjustment knob,
The cylinder is displaceably screwed to the main body.
A locking piece protrudes from an end of the plunger, and the locking piece is
Engageable between the end of the cylinder and the inner end of the adjustment knob
Noh. Plunger can be moved linearly in the axial direction
And promotes diversification of the cross-sectional shape of the mixing chamber to improve mixing efficiency.
To improve. Conduit to connect to plunger with simple configuration
Prevents rotation and twisting of pipes, and makes piping easy and compact
Can be done.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described below with reference to the drawings. In FIGS.
The mobile phase contains eluents 3 and 4 as mobile phases. Conduits 5 and 6 are connected to the solvent tanks 1 and 2, and the other end is connected to a mixer 7 serving as a mixing tank, and the amount of liquid sent is program-controlled by a microcomputer (not shown) therebetween. Liquid feed pumps 8 and 9 are interposed.

The mixer 7 has a main body 10 connected to conduits 5 and 6 and installed at a fixed position, a sleeve 11 on which a volume adjustment scale (not shown) is displayed on a peripheral surface, and an adjustment knob 12 as adjustment means. Have. Among them, a passage 13, 14 in communication with the guide <br/> pipe 5,6 to the inside of the main body 10 and the mixing chamber 15 is provided, the plunger guide 16 to the circumferential surface of the chamber 15 is arranged vertically I have.

In the upper part of the main body 10, a concave hole 17 communicating with the mixing chamber 15 is formed, and two seal rings 18 and 19 are fitted into the hole 17 in an overlapping manner. The O-ring 20 is mounted on the lower seal ring 18 among them.

The sleeve 11 is formed in a hollow cylindrical shape, and a screw portion 22 is provided on the inner surface of the hollow portion 21, and a flange portion 23 projects from the lower end. The flange portion 23 is fixed to the upper surface of the main body 10 via a plurality of bolts 24, and has a through hole 25 having a diameter substantially equal to the inner diameter of the plunger guide 16 in the center thereof.

The adjusting knob 12 is formed in a substantially cylindrical shape, and has a tapered surface 12a whose diameter is reduced downwardly formed on the lower half peripheral surface thereof. ing.

A hollow cylindrical cylinder 27 is provided in the concave chamber 26.
Is accommodated, and the lower end thereof projects from the lower end of the adjustment knob 12.
8 are formed. A flange 29 is projected from the upper end of the cylinder 27, and a screw 30 is screwed into the peripheral surface of the adjustment knob 12. The screw shaft end of the screw 30 is pressed against the end surface of the flange 29, and the cylinder 30 is pressed. Adjusting knob 27 12
It is connected integrally with.

A piston is inserted into the through hole 31 of the cylinder 27.
There straight rod and a cylindrical plunger 32 is accommodated, have locking piece 33 is protruded in its upper end, have appropriate tolerance for該片33 between the bottom and the flange portion 29 of the recessed chamber 26 And the upper end of the plunger 32 is latched.

The plunger 32 is formed of a cylindrical body approximately three times as long as the sleeve 11, and its lower peripheral surface is inserted into the through-hole 25 and the seal rings 18 and 19 so as to be slidable on the plunger guide 16. Mated.

A guide hole 34 communicating with the mixing chamber 15 is provided inside the plunger 32. One end of a conduit 35 is connected to an opening on the upper side thereof by appropriate means such as welding, and the other end is connected to a sample injector 36. It is connected to the.

In the drawing, reference numeral 37 denotes a column arranged in a column oven 38; 39, a detector such as a UV detector;
Reference numeral 0 denotes a conduit outlet hole formed on the upper surface of the adjustment knob 12.
It is desirable to provide a suitable stirring means such as a stirrer at the bottom of the mixing chamber 15.

FIG. 6 shows another embodiment of the present invention, in which the same reference numerals are used for portions corresponding to the above-described configuration. That is, in this embodiment, instead of connecting the conduits 5 and 6 directly to the mixer 7, the conduits 5 and 6 are connected to the switching valve 41, and the mixer 7 is connected to a predetermined port of the switching valve 41, and the switching valve 41 is connected.
It is characterized in that it can be applied to applications.

In particular, in this embodiment, the column 37 has an inner diameter of 1
When a microcolumn having a diameter of less than 1 mm is used, the flow rate accuracy of the liquid sending pump is limited in the configuration shown in FIG. 1 and it is difficult to obtain reproducibility of analysis. In the method of FIG. 6, the mixer 7 is replaced with a gradient initial solvent by the liquid sending pump 8, and the sample is injected from the injector 36, and the 6-way switching valve 41 is switched at the same time. As a result, the inside of the mixer 7 is gradually replaced by the final solvent of the gradient sent from the solution sending pump 9 and flows into the column 37, so that gradient analysis becomes possible. Conditions can be easily changed. Further, since the liquid sending pump 9 sends the liquid at a constant flow rate without changing the flow rate as shown in FIG. 1, the analysis reproducibility is also improved.

In the gradient mixer for a liquid chromatograph constructed as described above, a sleeve 21 is erected on the main body 10, a cylinder 27 is screwed into the sleeve 21, and an adjustment knob 12 is attached to an upper end of the cylinder 27. ing. Then, the plunger 32 attached to the adjustment knob 12 passes through the through hole 25 and the seal rings 18 and 19 and is inserted into the plunger guide 16, and the guide 1
6 and the bottom of the mixing chamber 15 form the volume of the mixing chamber 15.

Therefore, when the adjusting knob 12 is rotated around the axis, the cylinder 27 screwed inside the adjusting knob 12 rotates integrally with the adjusting knob 12 and is screwed or unscrewed into the sleeve 22 to move up and down. Then, the plunger 32 moves together with this, and the volume of the mixing chamber 15 changes.

In this case, since the locking piece 33 integral with the plunger 32 is assembled with a suitable allowance between the bottom of the concave chamber 26 and the flange 29, the plunger 32 can be adjusted by the adjusting knob 12. Therefore, the conduit 35 attached to the upper end of the plunger 32 does not rotate.

When a gradient analysis is performed using such a mixer, predetermined eluents 3, 4
And the liquid sending pump 8, based on the analysis conditions.
A program that defines the discharge amount of No. 9 or the feeding speed of the eluents 3 and 4 and the feeding amount or the feeding speed of the mixed solvent, gradient conditions, and the like is created, and is used as a micro program of a liquid chromatograph (not shown). Input to computer.

Next, the capacity of the mixing chamber 15 of the mixer 7, that is, the volume, is calculated based on the above analysis conditions, the gradient characteristics relating to the composition of the mobile phase, and the solvent replacement time. Adjust the capacity of the

As described above, the volume of the mixing chamber 15 is adjusted by rotating the adjusting knob 12, and at this time, the scale is displayed by referring to an adjustment scale (not shown) indicated on the peripheral surface of the sleeve 11. The adjustment knob 12 is adjusted to the lower end.
2 and 3 show the situation when the mixing chamber 15 is adjusted to a small capacity and a large capacity.

As described above, the adjustment can be performed simply and quickly by simply rotating the adjustment knob 12, and can be performed precisely and accurately by the screwing action of the screw portions 22, 28. Since the variable area of the capacity is set wide, the capacity in that area can be set arbitrarily.

When the analysis is started in such a situation and the liquid sending pumps 8 and 9 are driven, a predetermined amount of the eluents 3 and 4 are guided to the conduits 5 and 6 and sent to the mixer 7, and this is passed through the passage 7. It moves to the mixing chamber 15 via 13 and 14. Mixing room 15
Is adjusted to a predetermined volume, and the volume is maintained during the analysis. The eluents 3 and 4 that have flowed in are mixed, and this is stirred by a suitable stirrer (not shown) such as a stirrer to form a plunger. 32 is pushed out to the guide hole 34.

Thereafter, the mixed solvent moves through the guide hole 34 and is sent out to the conduit 35, and is guided from the tube 35 to the column 37 to elute each component of the sample. The change in the concentration of each component is detected by the detector 39. Is measured.

In this case, a concentration gradient is formed by the ratio of the amount of the eluents 3 and 4 flowing into the mixing chamber 15, and
The capacity of the mixing chamber 15 is related to the formation of the initial concentration of the gradient. For example, when the mixing chamber 15 is set to have a small volume as shown in FIG. 2, the eluents 3 and 4 mix quickly to form a uniform solvent concentration, while as shown in FIG. Is set to a large volume, the eluents 3 and 4 mix slowly, and it takes time to form a uniform solvent concentration.

Such a difference in the mixing state and a difference in the solvent concentration naturally affect the elution characteristics, and are expected to be related to the quality of the analysis. In order to confirm the above point, the inventor divided the volume of the mixing chamber 15 into large and small and performed the analysis. The analysis conditions are as follows. Sample; water-soluble vitamins Eluent A; 1-sodium hexanesulfonate aqueous solution (pH = 2 phosphoric acid) Eluent B; 1-sodium sodium hexanesulfonate aqueous solution (pH = 2 phosphoric acid) / acetonitrile = 20/80 column; Inertsil ODS-2 5 μm 150 × 4.6 mmφ gradient elution; A / B = 90/10 → (20 min) 70/30 flow rate; 1 ml / min detector; UV detector Peak component A: nicotinic acid, B: nicotinamide C, pyridoxal, D; pyridoxamine, E; pyridoxine, F;
Thiamine, G: folic acid, H: riboflavin, I: cyanocobalamin

FIGS. 4 and 5 are chromatograms showing the results of the above analysis. FIG. 4 shows that the volume of the mixing chamber 15 is 120 μL,
FIG. 5 shows a case where the setting is 830 μL. Among them, each peak component in FIG. 4 elutes faster overall than in FIG. 5, and the retention time is shortened. In addition, FIG. 4 shows no separation of G; folic acid, but FIG. 5 shows that G; folic acid is separated on the tail of the peak tailed by F; thiamine.

Therefore, these analysis results suggest the following points. In other words, when shortening the analysis time,
The capacity of the mixing chamber 15 may be set to a small volume, and the analysis time and the retention time of each component are estimated to be substantially inversely proportional to the capacity of the mixing chamber 15. Therefore, the capacity of the mixing chamber 15 is appropriately adjusted. Thus, the analysis time and the retention time of each component can be arbitrarily set or changed. Further, it is presumed that if the volume of the mixing chamber 15 is increased, the separation of each component becomes better. Therefore, by appropriately adjusting the volume of the mixing chamber 15 based on the separation state of the initial analysis, for example, Can be solved.

In the mixed flow method of the concentration gradient method as described above, one eluent is sent after a certain time at the start of the analysis, or one eluent is stopped during the analysis to remove the solvent. When changing the composition, the switching speed of the solvent is different by adjusting the volume of the mixing chamber 15, that is, if the mixing chamber 15 is adjusted to a small volume, the switching of elution is quick, while the mixing chamber 15 is adjusted to a large volume. If the volume is adjusted, the elution switching is performed slowly, so that the time for solvent replacement can be arbitrarily changed.

As described above, according to the present invention, the mixing capacity of the mixing chamber 15 can be varied with a simple structure, the solvent composition can be easily and precisely performed, and the analysis time and the retention time of each peak component can be arbitrarily changed. In addition, it is possible to improve non-separation of components.

[0034]

[Effect of the invention] The gradient mixer for liquid chromatography of the invention can slide the plunger as described above.
A cylinder to be supported is provided so as to be movable with the adjustment knob,
The cylinder is displaceably screwed into the body.
A locking piece is protruded from the end of the plunger,
A piece is engaged between the end of the cylinder and the inner end of the adjustment knob.
The plunger linearly in the axial direction.
Being movable makes it possible to diversify the cross-sectional shape of the mixing chamber
To improve mixing efficiency, and
Prevent rotation and twisting of the conduit connected to the
Is easily and compactly performed.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram showing a situation at the time of analysis using the present invention.

FIG. 2 is a cross-sectional view showing an embodiment of the present invention, in which a mixing chamber is adjusted to a small volume.

FIG. 3 is a cross-sectional view showing one embodiment of the present invention, in which a mixing chamber is adjusted to have a large capacity.

FIG. 4 is a chromatogram showing an analysis result obtained by adjusting a mixing chamber to a small volume.

FIG. 5 is a chromatogram showing an analysis result obtained by adjusting a mixing chamber to a large volume.

FIG. 6 is a view showing another embodiment of the present invention.

[Explanation of symbols]

 3, 4 Eluent (solvent) 7 Gradient mixer 10 Main body 12 Adjusting knob 15 Mixing chamber 32 Plunger

Continuation of the front page (72) Inventor Tomohito Watanabe 9-7 Tsukuba Spring, Inari-mae, Tsukuba City, Ibaraki Prefecture Second dormitory 411 (56) References JP-A-7-80820 (JP, A) JP-A-59- 160759 (JP, A) (58) Field surveyed (Int. Cl. ⁷ , DB name) G01N 30/34

Claims (1)

(57) [Scope of request for utility model registration] 1. A main body having a mixing chamber provided therein, and
A guide that is movably fitted and internally communicates with the mixing chamber.
A plunger with a hole formed on the outside of the plunger
Position and axially move the plunger via its rotational displacement
Adjustment knob and one end of the plunger
And a conduit communicating with the guide hole movably connected to the
In a liquid chromatograph gradient mixer in which the volume of the mixing chamber is adjustable via the displacement of the plunger, the plunger is slidably supported.
Cylinder is provided so as to be movable with the adjustment knob,
A screw is displaceably screwed into the main body, and the
A locking piece is protruded from the end of the lancer, and the locking piece is
An engageable arrangement between the end of the cylinder and the inner end of the adjustment knob
A gradient mixer for a liquid chromatograph , wherein the plunger is linearly movable in an axial direction .