JP3436853B2 - Method for producing packing material used for removal column - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention are use in the removal column for liquid chromatograph equipped with a circulation regression channel capable to remove residual sample components from the waste liquid in the post-analysis reused as eluent The present invention relates to a method for manufacturing a filler.

[0002]

2. Description of the Related Art FIG. 2 is an explanatory view showing a schematic configuration of a liquid chromatograph (so-called recycling system) having a circulation return flow channel.
Eluent storage tank 2 in which the eluent 3 is stored, and the eluent storage tank 2
A liquid feed pump 4 for pumping the eluent 3 in the channel, an injector 5 for introducing a sample into the eluent 3 pumped in the channel by the liquid pump 4, and a mobile phase after the sample is introduced. Separation column 6 for separating the sample, a detector 7 for detecting a sample component in the mobile phase flowing down through the separation column 6, and an eluent for removing the residual sample component from the waste liquid flowing down through the detector 7. By arranging at least the removal column 8 interposed for returning to the storage tank 2, the circulation returning flow path L is formed as a whole.

In this case, the removal column 8 is filled with a filler made of fine powdery activated carbon that adsorbs the sample components, and the waste liquid flows down through the removal column 8 to
As a result of being recycled and returned to the eluent storage tank 2 as a recovery liquid from which the residual sample components have been removed, it can be reused as an eluent.

[0004]

By the way, the liquid chromatograph 1 shown in FIG. 2 should theoretically be able to reuse the eluent.

However, in reality, in addition to the fine powder of activated carbon as a packing material, a sintered metal filter having pores having a relatively large pore size is used as a filter included in the removal column. A part of the packing material flows out from the container and becomes a mixed liquid, which is collected in the eluent storage tank 2.

As a result, when the eluent mixed with the recovered liquid reaches the separation column 6 side, the packing material of the separation column 6 is clogged to increase the pressure, and the separation column 6
However, the separation column is deteriorated and the separability is lowered, so that the separation column must be replaced with a new one, which is not practical.

[0007] The present invention has been made in view of the above problems found in the prior art, and its object is by improving the charging <br/> Hamazai removal column, accelerate deterioration of the separation column without and provides a method for producing a filler are use to removal column for liquid chromatograph equipped with a circulation regression passage can be stably used for a long time and without adversely affecting the chromatography To do.

[0008]

DISCLOSURE OF THE INVENTION The present invention is intended to achieve the above object, and the structural feature of the invention according to claim 1 is any one of coconut shell coal, coal, and rice husk coal. A firing process for obtaining activated carbon by firing one kind or a combination thereof appropriately at high temperature, and using the obtained activated carbon in methanol,
A separation step of separating the fine particle component and the granular component by stirring in a liquid of ethanol or acetone or a mixture thereof, and a drying step of drying the separated granular component to obtain granular activated carbon To produce a filler. In this case, the firing temperature in the firing step is preferably set in the range of 1500 to 3000 degrees Celsius as described in claim 2 .

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Filler obtained by the method of the present invention
Since a liquid chromatograph constructed by utilizing the above is constructed in the same manner as shown in FIG.
The same sites description are denoted by the same reference numerals as in FIG.

That is, the filling obtained by the method of the present invention.
A liquid chromatograph 1 configured by using an agent is provided with an eluent storage tank 2, a liquid delivery pump 4 for pumping the eluent 3 in the eluent storage tank 2 into a flow path, and a liquid delivery pump 4. An injector 5 that introduces a sample into the eluent 3 that is pressure-fed through the channel, and a separation column 6 that separates the mobile phase after the sample is introduced.
A detector 7 for detecting sample components in the mobile phase flowing down through the separation column 6; and residual sample components removed from the waste liquid flowing down through the detector 7 and returned to the eluent storage tank 2. For this reason, at least the removal column 8 interposed is provided to form the circulation return flow path L as a whole.

FIG. 1 schematically shows a main structure of a removal column 8 which constitutes the liquid chromatograph 1 in FIG. 2, and the removal column 8 is made of a hard glass material having a high pressure resistance. A tubular body 11 formed by using the tubular body 1 and the tubular body 1
A filler 12 to be filled in 1 and an inflow port 1 of a tubular body 11.
Packing 1 via a sealing plug 13 having an appropriate structure on the side of 1a
5 and the filter 17 disposed together with the tubular body 11 and the outlet 11b of the tubular body 11 through the sealing plug 14 as well as the packing 1
6 and at least a filter 18 arranged together, and the whole thereof is configured. Incidentally, reference numeral 21 in the drawing
Is a liquid feeding tube that constitutes the circulation return flow path L,
Shows a substantially C-shaped interposition ring used for surely connecting the tubular body 11 and the sealing plug 13 or 14 while ensuring liquid tightness.

The packing material 12 packed in the removal column 8
Is produced by the method of the present invention described below.

That is, the filler 12 is coconut shell charcoal,
Of coal and rice husk charcoal, any one kind or a suitable combination thereof is fired at a high temperature in the range of about 1500 to 3000 degrees Celsius, more preferably in the range of 1700 to 2700 degrees Celsius to obtain activated carbon. While the activated carbon is stirred in a liquid of methanol or ethanol, for example, a separation step of separating the granular components by allowing the floating fine particle components to flow and leaving the granular components remaining, and the separated granular components for 1 week It is manufactured through a drying process in which granular activated carbon is obtained by drying in the shade for a while.

In this case, as the activated carbon, activated carbon made of coal obtained by firing coal at a high temperature is porous, that is, excellent in adsorption ability, and can be particularly preferably used.

Further, the granular activated carbon obtained after being separated through the above separation step prevents clogging and at the same time reliably adsorbs the residual sample components which are organic substances,
A particle size of about 50 to 120 mesh can be preferably used.

On the other hand, as the filters 17 and 18, a porous ceramic filter formed by a glass sintered material obtained by sintering alumina glass powder can be preferably used.

In this case, the porous ceramic filter has fine pores having a pore diameter in the range of 0.5 to 5 μm, more preferably 0.5 to 3 μm, from the viewpoint of preventing the filler 12 from flowing out. It is desirable to use the one with holes.

Next, the filler 1 obtained by the method of the present invention
Explain the operation of the removal column 8 packed with 2
For example, as shown in FIG. 2, the waste liquid flowing down through the detector 7 passes through the filter 17 arranged at the inflow port 11a of the cylindrical body 11 and comes into contact with the filler 12 produced by the method of the present invention. To reach.

At this time, since the filler 12 made of granular activated carbon is used, the residual sample components in the waste liquid can be surely adsorbed and removed, and thus the residual sample components are not contained. The liquid, that is, the original eluent is regenerated and flows out through the filter 18 arranged at the outlet 11b.

Moreover, the filter 18 has a pore size of 0.5.
Since it is formed by a porous ceramic filter having fine pores of about 5 μm, it is possible to reliably prevent the granular activated carbon with a particle size of about 50 to 120 mesh from flowing out, so that it can be used as an eluent after regeneration. It can be collected in the eluent storage tank 2 without containing the filler 12.

Therefore, even if the recovered liquid reaches the separation column 6 again as the eluent 3, it can be permeated without causing clogging of the packing material, so that performance deterioration due to pressure increase does not occur. The separation column 6 can be practically used for a long period of time while maintaining the initial resolution.

Moreover, because the performance of the separation column 6 does not deteriorate, the eluent can be reused without adversely affecting the obtained chromatography.

Further, the removal column 8 itself is also filled with the packing material 12
Since granular activated carbon having a particle size of about 50 to 120 mesh is used in combination with the presence of filters 17 and 18 which are porous ceramic filters, they can be practically used for several years before being used. You can continue.

[0024]

The filler obtained by the method of the present invention is filled.
By interposing the removal column, it is possible to reliably remove the residual sample components from the waste liquid and to recover it as a regenerated eluent containing no packing material, thus eliminating the need for waste liquid treatment. It is possible to eliminate the exposure of the person in charge of the experiment to the organic solvent contained in the liquid and the factors that cause pollution, and it is possible to effectively reduce the amount of the eluent used and greatly reduce the running cost. Can be contributed.

Moreover, even when the recovered liquid is used as the eluent, the packing material in the separation column can be permeated without causing clogging, so that the initial separation can be carried out without causing performance deterioration due to pressure increase. Not only can the separation column be practically used for a long period of time while maintaining its performance, but it can also be prevented from adversely affecting the chromatography.

Further, since the removal column itself also uses the granular activated carbon as a packing material, in combination with the presence of the filter which is a porous ceramic filter, it exhibits practical performance for several years and is stable. Can be used.

[Brief description of drawings]

FIG. 1 is an explanatory view schematically showing a cross-sectional structure of a removal column filled with a packing material obtained by the method of the present invention, omitting a part thereof.

FIG. 2 is an overall configuration diagram showing an outline of a liquid chromatograph provided with a circulation return flow channel.

[Explanation of symbols]

1 Liquid chromatograph 2 Eluent storage tank 3 eluent 4 Liquid feed pump 5 injectors 6 Separation column 7 detector 8 Removal column 11 tubular body 11a Inlet 11b Outlet 12 Filler 13,14 Sealing plug 15,16 packing 17,18 filter 21 Liquid transfer tube 22 Interposer ring L circulation return flow path

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Claims (2)

(57) [Claims] 1. A calcination step of activating coconut shell charcoal, coal or rice husk charcoal to obtain activated carbon by high-temperature firing of any one kind or a combination thereof, and the obtained activated carbon is selected from one of methanol, ethanol and acetone. The filler is manufactured through a separation step of stirring in the liquid or the mixed solution thereof to separate the fine particle component and the granular component, and a drying step of drying the separated granular component to obtain granular activated carbon. A method for producing a packing material for use in a removal column, comprising: 2. The firing temperature in the firing step is 1 degree Celsius.
The process according to claim 1, wherein the filler, which is a range of 500 to 3000 degrees.