JPH0989861A - Column unit for gas chromatography - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a highly reliable column unit for gas chromatography in which an inexpensive plastic column can be used. SOLUTION: A tubular enclosed container 12 contains a plurality of stationary phase extraction cartridges 111 -115 connected detachably in series with the moving phase introduction port 11a and moving phase feeding port 11b of each stationary phase extraction cartridge communicating with the outside. Each stationary phase extraction cartridge 111 -115 contained in the tubular enclosed container 12 is provided, at the coupling part thereof, with a seal mechanism 2 for hermetically sealing the coupling part against the outside of stationary phase extraction cartridge.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid chromatography column device, and more particularly to a liquid chromatography column device suitable for high performance liquid chromatography.

[0002]

2. Description of the Related Art Chromatography has hitherto been carried out in the equilibrium field formed by two phases called a stationary phase and a mobile phase, in which various compounds interact with each other (adsorption, partition, ion exchange, molecule). It is generally widely used as a method for separating and quantifying the difference based on the difference in size and the like.

Among these, liquid chromatography uses a liquid as a mobile phase, and a liquid chromatograph is an apparatus that automates this. In addition, in this device, which is a liquid chromatograph, a liquid that is a mobile phase is sent at high pressure to shorten the analysis time, which is called a high performance liquid chromatograph (HPLC). FIG. 9 shows a schematic configuration of a high performance liquid chromatograph.

In FIG. 9, reference numeral 101 is a mobile phase W.
The reference numeral 102 denotes a liquid feed pump. Reference numeral 103 indicates a sample injector, reference numeral 104 indicates a column (substance separation unit), and reference numeral 105 indicates a detector.

Of these, in actual measurement, for example, a solution containing a sample of several microliters to several hundreds of microliters is introduced into the column 104 from the sample injector 103. The liquid feed pump 102 forms the center of the apparatus, and generally a reciprocating plunger pump is often used. In this case, the liquid feed pump 102 has been devised to quantitatively feed the mobile phase, and economic efficiency and maintainability are also emphasized.

The detector 105 is, for example, an ultraviolet spectrophotometer for measuring the ultraviolet absorption intensity of a compound, and is equipped with a flow cell of about 8 to 20 [microliter]. There are a differential refractometer for measuring changes in refractive index, a fluorophotometer for measuring fluorescence, and the like. Sometimes an electrochemical detector is also used to quantify the amount of compound in ng-μg.

Further, the column 104 has, for example, an inner diameter of 1 to 6
A stainless steel pipe having a length of [mm] and a length of 5 to 30 [cm], which is usually densely filled with a fine filler (stationary phase) having a diameter of 3 to 10 [μm]. This kind of column 104
Is stored in a thermostat (column oven) 104A,
It is kept at a constant temperature.

[0008] Further, such a device is characterized in that a compound having insufficient volatility or a compound which is thermally unstable can be easily analyzed. Further, the separated compound can be easily separated and excellent in quantification. It has advantages that other separation methods do not have.

[0009]

However, in the above-mentioned conventional example, the column 104 is used for highly accurate measurement.
Since an expensive stainless steel one (30,000 yen to 100,000 yen: as of August 1, 1995) is used as a column, if you prepare several types of columns for multiple purposes, many measurements will be made each time. There was an inconvenience that it was expensive.

In order to improve such inconvenience, an inexpensive plastic material is also commercially available, but it has low reliability against pressure fluctuation during measurement due to its low pressure resistance. For this reason, there is a disadvantage that expensive stainless steel materials must be used for the separation and analysis of particularly important substances.

[0011]

The object of the present invention is to improve the inconvenience of the conventional example, and in particular, even if the column is made of an inexpensive plastic, it enables highly accurate measurement without damage and pressure fluctuation during the measurement. It is an object of the present invention to provide a highly reliable column apparatus for liquid chromatography that can effectively cope with the above.

[0012]

According to a first aspect of the present invention, a plurality of solid phase extraction cartridges detachably connected in series are provided, and the mobile phase inlet and the mobile phase outlet of each solid phase extraction cartridge are externally connected. It is equipped with a cylindrical airtight container that is stored and equipped in communication with the. A structure is provided in the vicinity of the connecting portion of each solid phase extraction cartridge mounted in the cylindrical closed container, and a sealing mechanism for sealing the connecting portion to the outside of the solid phase extraction cartridge. .

When extracting a plurality of components in a sample, each of a plurality of solid phase extraction cartridges is individually filled with a packing that easily captures the intended component (many are commercially available in a filled state). ), And then equip it in a cylindrical closed container. In this case, the solid-phase extraction cartridge is sequentially housed together with the sealing mechanism, and the whole is integrated.

Next, the cylindrical closed container is incorporated into the component extraction system (FIG. 2), and then the system is put into operation. As a result, the inside of each solid phase extraction cartridge is
The pressure is about 20 to 30 [Kg / cm ² ], but since the solid phase extraction cartridges are covered by the cylindrical hermetically sealed container surrounding the solid phase extraction cartridges, a pressure of this level and fluctuation thereof Has sufficient pressure resistance.

By continuing such a state for a predetermined time, a plurality of components corresponding to the function of the packing are individually and simultaneously collected in each solid phase extraction cartridge. Then, the operation of the system is stopped, and each solid phase extraction cartridge is taken out from the cylindrical closed container. Then, the collected components are easily extracted with a predetermined solvent.

According to a second aspect of the invention, in the liquid chromatography column apparatus according to the first aspect,
A configuration in which a cylindrical closed container is divided into a plurality of container body portions for each solid phase extraction cartridge, and the plurality of divided container body portions are connected to each other while maintaining a sealed state. Is taking. Therefore, the number and position (linkage order) of the solid phase extraction cartridges can be grasped, so that the solid phase extraction cartridges can be easily managed, the component extraction work can be carried out more quickly and smoothly, and the component leakage can be completely prevented. Can be eliminated.

According to a third aspect of the present invention, the above-mentioned sealing mechanism is provided around a connecting portion of a plurality of solid phase extraction cartridges, a cylindrical member, both end portions of the cylindrical member and the solid members. The method is that it is configured with a seal member mounted between the phase extraction cartridge and the phase extraction cartridge. Therefore, it is possible to completely eliminate the component leakage from the connecting portion between the solid phase extraction cartridges, and the reliability of the measurement technique and the apparatus is further improved. This aims to achieve the above-mentioned object.

[0018]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of a liquid chromatography column device according to the present invention will be described below.

[0019]

[First Embodiment] A first embodiment will be described with reference to FIGS. Here, the same reference numerals are used for the same constituent members as those in the conventional example shown in FIG.

First, FIG. 2 shows a schematic explanatory view of a high performance liquid chromatograph. In FIG. 2, reference numeral 1 indicates a column device for liquid chromatography according to the present invention. On the sample introduction side (left side in FIG. 2) of the column device 1, a mobile phase storage unit 101 for storing a predetermined liquid as a mobile phase W.
A liquid feed pump 102 forcibly feeding the mobile phase W in the mobile phase storage unit 101 to the column device 1 described above; and a predetermined sample together with the mobile phase W from the liquid feed pump 102 in the column device 1. The sample injector 103 for injection is sequentially connected in series. Further, a detector 105 for quantitatively detecting the substance in the mobile phase is equipped on the sample delivery side (right side in FIG. 2) of the column device 1.

In the first embodiment, the column device 1 is provided with _five solid phase extraction cartridges 11 ₁ , 11 _{2 to} 11 ₅ made of plastic as shown in FIG. Can be any number. The solid-phase extraction cartridges 11 _{1 to} 11 ₅ in FIG. 1 are connected to each other in series and detachably with their center lines coaxially arranged. In addition, each of the solid phase extraction cartridges 11 _{1 to} 11 ₅
Has a mobile phase inlet 11a and a mobile phase outlet 11b at both ends.

[0022] Then, solid-phase extraction cartridge 11 located in the mobile phase inlet port 11a and the other end portion of the solid-phase extraction cartridge 11 ₁ located at one end of the linked solid-phase extraction cartridge 11 ₁ to 11 _{5 5} Of the solid-phase extraction cartridges 11 _1-
11 _5, the ambient is equipped housed in close contact with the body portion into the cylindrical closed vessel 12 (in the figure in part by that can removably are described by a gap).

Each of the solid phase extraction cartridges 11 _{1 to} 11
Reference numeral ₅ denotes the internal mobile phase inlet 11a side and the mobile phase outlet 11
A filter 11F is provided on the b side, and a predetermined filler 11G is filled between the filters 11F.

Here, the cylindrical closed container 12 is composed of six container body portions 13 to 18. Of these, the first container body 13 is disposed on the mobile phase introduction side,
Further, the sixth container body 18 is arranged on the mobile phase delivery side. Then, between the first container body portion 13 and the sixth container body portion 18, the same second to fifth portions are formed.
The container body parts 14 to 17 are equipped.

The first container body 13 has a mobile phase introducing portion 13A at the center of the upper end of FIG. 1, and also has a counterbore-like recess 13B opened downward in FIG. 1 and the counterbore-like recess 1.
3B is provided with a recessed portion 13Ba provided at the center of the bottom portion, and further, a connecting male screw portion 13C is formed on the outer periphery of the spot facing recessed portion 13B. Among these, the mobile phase introducing portion 13A is an introduction guide hole 13Aa which is continuous with the above-mentioned recess 13Ba at the central axis portion of the first container body 13.
And a piping piece 13Ab screwed from the outside into the introduction guide hole 13Aa.

The solid-phase extraction cartridge 11 ₁ described above is disposed and equipped in the recess 13Ba of the first container body 13 via the cylindrical cover 13D. In this case, a circular groove is formed around the introduction guide hole 13Aa on the concave portion 13Ba side of the first container body 13 (corresponding to the periphery of the mobile phase introduction port 11a of the solid phase extraction cartridge 11 ₁ ). The mobile phase introduction port 11a of the solid phase extraction cartridge 11 ₁ described above is inserted therein. Therefore, the mobile phase and the sample introduced into the mobile phase introducing section 13A are directly introduced into the solid phase extraction cartridges 11 _{1 to} 11 ₅ in the cylindrical closed container 12.

The second container body 14 is provided with a female screw portion 14A on the upper end side in FIG. 1 to be screwed into the connecting male screw portion 13C of the first container body 13, and on the opposite side (see FIG. 1). The lower end side) is provided with a male thread portion 14C for connection which is the same as the male thread portion 13C for connection of the first container body 13 described above, and a through hole 14D for equipment for equipping the solid phase extraction cartridge 11 ₂ in the central portion. Is equipped with.

Further, the central portion of the second container body 14 surrounded by the female screw portion 14A is projected toward the counterbore-shaped recess 13B of the first container body 13 described above. A hermetic seal member S is provided between the periphery of the protrusion 14Aa of the second container body 14 and the side wall of the counterbore-shaped recess 13B described above.

The second container body 14 is provided with a counterbore-shaped recess 14B in the central portion of the lower end in FIG. 1 as in the case of the first container body 13 described above. The counterbore-shaped recess 14B has a recess 14B at the center thereof.
a is formed, and the above-described equipment through hole 14D is formed at the center of the recess 14Ba, and the second solid phase extraction cartridge 11 ₂ is housed in the equipment through hole 14D and the recess 14Ba. It has become so.

At the connecting portion between the first solid-phase extraction cartridge 11 ₁ and the second solid-phase extraction cartridge 11 ₂ described above, a seal mechanism 2 for sealing the connecting portion to the outside is provided. There is. The sealing mechanism 2 includes a cylindrical member 2A arranged in the equipment through hole 14D around the connecting portion of the first and second solid phase extraction cartridges.
When the sealing member 2 that is provided between the end portions and the solid-phase extraction cartridge 11 _1, 11 ₂ of the cylindrical member 2A
B and 2C.

Therefore, by the action of the sealing mechanism 2, the inside air and the outside air of the connecting portion of the solid phase extraction cartridges 11 ₁ and 11 ₂ are shut off, and the solid phase extraction cartridges 1 are
Leakage of the components extracted at 1 ₁ and 11 ₂ is prevented.

Hereinafter, the third to fifth container body parts 15 to 1 will be described.
7 is also formed in exactly the same manner as the second container body 14 and functions in the same manner. Reference numeral 11 ₃ , 1
1 ₄ . 11 _5, the container main body portion 15 to 17 of the third to fifth
2 shows a solid-phase extraction cartridge housed in each part of FIG.
The solid phase extraction cartridges 11 ₂ , 11 ₃ , 11 ₄ , etc. in the third to fifth container body portions 15 to 17. 11
Each of the connecting portions of ₅ is also equipped with the above-mentioned sealing mechanism 2.

A sixth container body 18 is provided at the lower end of FIG. This sixth container body 18
1, the lower end surface of FIG. 1 is a flat surface, and the mobile phase delivery unit 18A is provided in the center thereof. This mobile phase transmitter 18
A is composed of a delivery guide hole 18Aa formed in the central axis portion of the sixth container body 18, and a pipe piece 18Ab externally screwed to the delivery guide hole 18Aa. The upper end portion of the sixth container body portion 18 in FIG. 1 is configured exactly the same as the upper end portions of the second to fifth container body portions 14 to 17 described above.

Inside the delivery guide hole 18Aa described above, the fifth solid phase extraction cartridge 11 ₅ described above is
The mobile phase delivery port 11b portion of is inserted tightly. Therefore, the fifth from the solid phase extraction cartridge 11 _5, the mobile phase is adapted to be smoothly fed out to the outside without leaking into the cylindrical closed vessel 12.
Further, the sealing portions S are also provided on the engaging portions of the second to sixth container body portions 14 to 18 as in the case of the engagement of the first to second container body portions 13 to 14 described above. Has been done.

Next, the operation and the like of the first embodiment will be described. First, when extracting a plurality of components from a sample, each solid phase extraction cartridge 11 _{1 to} 11 ₅ was filled with a filling material that easily captures the intended component (many are commercially available in a filled state). After that, as shown in FIG. 1, the equipment is housed in the cylindrical closed container 12. In the embodiment of FIG. 1, five types of component detection are executed at the same time.

In this case, the second to sixth container body parts 1
The hermetic seal member S is previously attached to 4 to 18. The solid-phase extraction cartridges 11 _{1 to} 11 ₅ are individually housed together with the sealing mechanism 2 in each of the first container body 13 to the fifth container body 17, and then the first container body 1
The third to fifth container body parts 17 are sequentially screwed and connected, and finally the sixth container body part 18 is screwed and integrated as a whole as shown in FIG.

Next, solid phase extraction cartridges 11 _{1 to} 11
_The tubular closed container 12 containing ₅ is incorporated into the system of FIG. 2, and then the system is operated. As a result, first, the mobile phase W is pumped from the liquid feed pump 102 and sent into the column apparatus 1, and at the same time, the solution containing the sample is also sent from the sample injector 103 together with the mobile phase W to the column apparatus 1.
It is sent in. And each solid phase extraction cartridge 1
1 ₁ to 11 inside the _5, 20-30 [Kg / cm ^2] is the pressure before and after the solid-phase extraction cartridge 11 ₁ to 1
Since the periphery of ₁₅ is abutted and covered by the cylindrical hermetically sealed container 12, sufficient pressure resistance is maintained against this level of pressure and its fluctuation. The symbol P _W indicates the inflow and outflow directions of the mobile phase W.

By continuing such a state for a predetermined time, a plurality of components corresponding to the function of the packing are individually and simultaneously collected in each solid phase extraction cartridge 11 _{1 to} 11 ₅ . After that, the operation of the system is stopped in FIG. 2 and the cylindrical closed container 12 is disassembled into the container body parts 13 to 18, so that the solid phase extraction cartridges 11 _{1 to} 11 ₅ can be taken out. Then, the collected components are easily extracted with a predetermined solvent.

As described above, in the first embodiment shown in FIGS. 1 and 2, an inexpensive solid phase extraction cartridge made of plastic (about 400 to 800 yen; August 1, 1995) (Currently) can be used to extract the same components as in the case of an extremely expensive stainless steel column, and it is possible to extract five types of components in a sample at the same time with a single measurement. Since the time can be greatly shortened, and in particular, a plurality of types of components can be extracted at the same time, new components can be extracted at the same time, and the cylindrical closed container 12 can be repeatedly used. There is an advantage that the time and labor required for the component extraction can be significantly reduced.

Further, in the above-mentioned embodiment, since the cylindrical closed container 12 has a structure capable of being disassembled into a plurality of container body portions 13 to 18 corresponding to the solid phase extraction cartridges 11 _{1 to} 11 ₅ , Since the number and position (linking order) of the solid phase extraction cartridges can be grasped, the solid phase extraction cartridges can be easily managed, and in this respect, the component extraction work can be carried out more quickly and smoothly than the conventional one. There are advantages.

[0041] Further, in the above embodiment, equipped at both ends of the solid-phase extraction on the connecting portion of the cartridge 11 ₁ to 11 ₅ provided with a sealing mechanism, the sealing mechanism and the cylindrical member Each cylindrical member since it is configured by the the seal member, a component leaking from the connecting portion of the solid-phase extraction cartridge 11 ₁ to 11 ₅ can be completely eliminated, thereby further improve the reliability of the measurement techniques and equipment There is an advantage that you can.

[0042]

[Second Embodiment] Next, a second embodiment will be described with reference to FIG. Here, the same reference numerals are used for the same components as those in the embodiment of FIG. 1 described above.
The second embodiment shown in FIG. 3 is a cylindrical closed container 22 obtained by improving the cylindrical closed container 12 shown in FIG. 1 described above.

The cylindrical closed container 22 is composed of the first container body 23 to the sixth container body 28 as in the case of FIG. 1 described above. Of these, the first container body portion 23 has the side wall portion of the counterbore-shaped recess 13B of the first container body portion 13 in FIG. 1 described above removed, and the outside of the first container body portion 23 by that much. Figure 1 whose diameter is described above
It is set to be significantly smaller than the one. Code 2
3C shows a male screw portion for connection. This first container body 2
3 is the same as the first configuration in FIG. 1 described above.
The container main body 13 is formed in the same manner as the container main body 13, the mobile phase introducing portion 13A is provided, and the solid phase extraction cartridge 11 ₁ is also housed in the recess 23Ba through the cylindrical cover 13D.

The second container body 24 has an internal thread 24A at the upper end of FIG. 3 corresponding to the above-mentioned connecting male screw 23C, and the lower end of FIG. 3 has the above-mentioned first container. Like the main body portion 23, the connecting male screw portion 23C is provided. Other configurations are the same as those of the second container body 14 in FIG. 1 described above.

Third to fifth container body parts 25 to 27
₃ , the solid phase extraction cartridges 11 ₃ , 11 ₄ , and 11 ₅ are detachably housed in the same manner as the second container body 24 as shown in FIG. Equipped.

In the sixth container body 28, the lower end surface of FIG. 3 is a flat surface, and like the case of FIG. 1 described above,
A mobile phase sending unit 18A is provided at the center thereof.
The upper end portion of the sixth container body portion 28 in FIG. 3 is configured exactly the same as the upper end portions of the second to fifth container body portions 24 to 27 described above. Other configurations are the same as those in the case of FIG. 1 described above.

Even in this way, the above-mentioned FIGS.
In addition to having the same effects as the embodiment described above, there is an advantage that the cylindrical closed container 22 can be made smaller and lighter, and the portability is good.

[0048]

[Modification] Next, a modification of the second embodiment shown in FIG. 3 will be described with reference to FIGS. Here, the same reference numerals are used for the same constituent members as those in FIG. 3 described above.

FIG. 4 shows a modification of the first container body 23 in FIG. 3 described above. The first container body 33 shown in FIG. 4 has a cylindrical cover 13D shown in FIG.
With removing the solid-phase extraction cartridge 11 ₁ is housed directly in the recess 33Ba, further an inner bottom surface of the recess 33Ba (the inner upper surface in FIG. 4) and the solid-phase extraction cartridge 11 ₁
The feature is that an O-ring 33Bb for sealing is provided between and. In this case, the inner diameter of the recess 33Ba is set to a size suitable for the solid phase extraction cartridge 11 ₁ . Other configurations are the same as those of the first container body 23 in FIG. 3 described above. Even in this case, it is possible to obtain the same effects as those in the case of FIG. 3 described above, and it is possible to reduce the number of parts.

Next, referring to FIG. 5A and FIG.
A modified example of the sixth container body 28 in FIG. Of these, in the sixth container main body portion 38 shown in FIG. 5 (A), the periphery of the mobile phase outlet 11b located inside the mobile phase delivery portion 18A described above is formed into a conical shape. The present invention is characterized in that an annular seal member 38S is provided in a mobile phase outlet / accommodation portion 38a that is formed in a circular shape.

[0051] Further, FIG. 5, 6 of the container body portion 39 (B), the between the lower end surface of the main body portion of the solid-phase extraction cartridge 11 ₅ and 6 of the container body portion 39, an annular seal member 3
The feature is that it is equipped with 9S. All other configurations are the same as those of the sixth container body 28 shown in FIG. 3 described above.

Even in this case, in addition to the same function as in the case of FIG. 3 described above, there is an advantage that the sealing function is particularly strengthened and the reliability of the entire apparatus can be improved.

Next, FIGS. 6A to 6D show modified examples of the seal mechanism 2 provided inside the second container body 24 to the fifth container body 27 described above. .

Of these, the seal mechanism 20 shown in FIG.
Reference numeral 1 denotes two annular seal members 201A and 201B, and a cross section U holding the annular seal members 201A and 201B.
It is configured by a character-shaped seal holding member 201C. The seal holding member 201C is equipped with its opening facing upward so as to protect the solid-phase extraction cartridge (for example, 11 ₁ ) located on the upper side. Further, the one annular seal member 201A is formed in a V-shaped cross section, and the through hole of the seal holding member 201C is also widened in a skirt shape in accordance with this.

The other annular seal member 201B is
It is provided in a state in which it is formed in a T-shaped cross section and the upper end portion is fitted to the lower side of the one annular seal member 201A having the C-shaped cross section described above. Therefore, the container body portions 23-2
Simultaneously with the screw assembly of 8, the constituent members of each part of the seal mechanism 201 are compressed so that the sealing function is exerted as a whole.

A seal mechanism 202 shown in FIG. 6B has a tubular seal member 202A and the tubular seal member 202A.
Two solid phase extraction cartridges (eg 11
₁ and 11 ₂ ), the sealing O-rings 202a and 202b separately provided on both sides with the connecting portion sandwiched therebetween, and the seal holding member 20 having a U-shaped cross section for holding the tubular sealing member 202A.
2B and.

In this case, in the cylindrical seal member 202A, the center of the outer periphery projects outward and forms a mountain shape, whereby an annular inclined surface is formed on the outer periphery. Corresponding corners of the seal holding member 202B, the second container body 24, and the like described above are cut off obliquely according to the shape of the tubular seal member 202A. Therefore, at the same time as the container main body portions 23 to 28 are screwed and assembled, the constituent members of the respective portions of the seal mechanism 202 are compressed, whereby the sealing function is exerted as a whole.

A sealing mechanism 203 shown in FIG. 6C has a tubular sealing member 203A and the tubular sealing member 203A.
And a seal holding member 203B having a U-shaped cross section. In this case, the tubular seal member 203A
Has a mountain-like shape in which the center of the outer peripheral surface thereof projects to the outside, and thereby an annular inclined surface is formed vertically on the outer periphery thereof. Corresponding corners of the seal holding member 203B, the second container body 24, and the like described above are cut off obliquely according to the shape of the tubular seal member 203A. Therefore, at the same time when the container main bodies 23 to 28 are screwed and assembled, the constituent members of the respective parts of the seal mechanism 202 are compressed,
As a result, the sealing function is exerted as a whole.

The seal mechanism 204 shown in FIG. 6D is composed of a single cylindrical seal member 204A.
In this case, in the cylindrical seal member 204A, the outer periphery of the lower end portion is cut into an inverted conical shape in the figure, and correspondingly corresponding corner portions of the second container body portion 24 and the like described above are cut obliquely. A cutout portion 204a is provided. For this reason, the tubular seal member 204A is compressed in the excision portion 204a at the same time when the container main body portions 23 to 28 are assembled by screwing, whereby the sealing function is exerted as a whole.

In this way as well, in addition to having the same effect as the sealing mechanism 2 in FIG. 3 described above, the whole connecting portion is uniformly and planarly sealed in each solid phase extraction cartridge. There is an advantage that the sealing effect of the connecting portion can be further enhanced.

[0061]

[Third Embodiment] Next, a third embodiment will be described with reference to FIG. Here, the same reference numerals are used for the same components as those in the embodiment of FIG. 1 described above.
In the third embodiment shown in FIG. 7, the cylindrical closed container 12 shown in FIG. 1 described above is further improved into a cylindrical closed container 32.

Cylindrical closed container 3 according to the third embodiment
2 is six container body parts 3 as in the case of FIG. 1 described above.
3 to 38, and these are integrated by four long screws (six may be used) 39 evenly arranged on the circumference. Of these, the first container body 33 is arranged on the mobile phase introduction side, and the sixth container body 38 is arranged on the mobile phase delivery side. Then, between the first container body portion 33 and the sixth container body portion 38, the container body portions of the same second to fifth container body portions 34 to 37 are provided.

The first container body 33 has a structure in which a mobile phase introducing portion 13A is provided at the center of the upper end portion of FIG. 1 and a concave portion 33A opened downward in FIG. Among these, the mobile phase introducing portion 13A is the introduction guide hole 1 which is continuous with the above-mentioned concave portion 33A at the central axis portion of the first container body 33.
3Aa and a pipe piece 13Ab screwed into the introduction guide hole 13Aa from the outside.

Then, in the recess 33A of the first container body 33, the above-mentioned solid phase extraction cartridge 11 ₁ is arranged and equipped via the cylindrical cover 13D. In this case, around the introduction guide hole 13Aa on the recess 33A side of the first container body 33 (the solid phase extraction cartridge 11
_A circular groove is formed around the mobile phase introduction port 11a of _{1), and} the mobile phase introduction port 11a of the solid phase extraction cartridge 11 ₁ described above is inserted in the circular groove. . Therefore, the mobile phase and the sample introduced into the mobile phase introducing section 13A are directly introduced into the solid phase extraction cartridges 11 _{1 to} 11 ₅ in the cylindrical closed container 12.

The second container body 34 has a through hole 34D for mounting the solid-phase extraction cartridge 11 ₂ at the center thereof. And this equipment through hole 3
The second solid-phase extraction cartridge 11 ₂ is housed in the 4D via the cartridge holding cylinder 34H.

In this case, the lower end of the _first solid phase extraction cartridge 11 ₁ in FIG. 7 (the mobile phase outlet 11
The portion b) is fitted and arranged in the cartridge holding cylinder 34H. That is, in FIG. 7, the cartridge holding cylinder 34
It has a feature in that the connecting portion between the solid phase extraction cartridges described above is arranged in the H. Reference numerals 2B and 2C indicate O-rings for sealing the connecting portion.

Therefore, due to the sealing action of the O-rings 2B and 2C, the solid phase extraction cartridges 11 ₁ and 11 _{2 are}
The inside and the outside of the connecting portion of the solid phase extraction cartridge are cut off from each other to prevent leakage of the components extracted by the solid phase extraction cartridges 11 ₁ and 11 ₂ .

Hereinafter, the third to fifth container body portions 35 to 3 will be described.
7 is also formed in exactly the same manner as the second container body 34 and functions in the same manner. Reference numeral 11 ₃ , 1
1 ₄ . 11 _5, the container body of the third to fifth 35-37
2 shows a solid-phase extraction cartridge housed in each part of FIG.
In addition, the solid phase extraction cartridges 11 ₃ , 11 ₄ , ... In the third to fifth container body portions 35 to 37. 11 ₅ is equipped individually in each container body 35 to 37 via a cartridge holding barrel 35H～37H.

A sixth container body 38 is provided at the lower end of FIG. This sixth container body 38
1, the lower end surface of FIG. 1 is a flat surface, and the mobile phase delivery unit 18A is provided in the center thereof. This mobile phase transmitter 18
A is composed of a delivery guide hole 18Aa formed in the central axis portion of the sixth container body 38, and a pipe piece 18Ab screwed to the delivery guide hole 18Aa from the outside. The upper end portion of the sixth container body portion 38 in FIG. 1 is configured exactly the same as the upper end portions of the second to fifth container body portions 34 to 37 described above.

Inside the delivery guide hole 18Aa described above, the fifth solid phase extraction cartridge 11 ₅ described above is
The mobile phase delivery port 11b portion of is inserted tightly. Therefore, the fifth from the solid phase extraction cartridge 11 _5, the mobile phase is adapted to be smoothly fed out to the outside without leaking into the cylindrical closed vessel 32.

The first to sixth container body portions 13 to
An O-ring 32S for sealing is provided between the 18 members. Further, the first to sixth container body portions 13 to
Between the 18 parts, inside the O-ring 32S for sealing,
Engaging concave portions 32a and convex portions 32b are respectively provided, whereby the first to sixth container body portions 13 to 1 are provided.
The integration of 8 is robust.

Even in this manner, the above-described FIGS.
Embodiments and in addition to having a same effect, four long screws 39 which particularly mentioned above the built-in and removal of the cylindrical closed vessel 32 of the solid-phase extraction cartridge 11 ₁ to 11 ₅
This has the advantage that the workability can be further improved by performing only the operation of.

[0073]

Fourth Embodiment Next, a fourth embodiment will be described with reference to FIG. Here, the same reference numerals are used for the same components as those in the embodiment of FIG. 1 described above.
The third embodiment shown in FIG. 8 is a cylindrical closed container 42 obtained by further improving the cylindrical closed container 12 shown in FIG.

Cylindrical closed container 4 according to the fourth embodiment
2 is different from the case of FIG. 1 described above in that the solid-phase extraction cartridges 11 _{1 to} 11 ₅ are accommodated in a single cylindrical container body 43.

This will be described in more detail below. The tubular closed container 42 according to the fourth embodiment is a single tubular container body 4
3, the first and second cap mechanisms 44 and 45 screwed to both ends of the tubular container body 43, and the solid-phase extraction cartridges 11 _{1 to} 11 ₅ described above as a whole. Cartridge fixed body 4 fixed and held at both ends of the
6, 47 and the solid phase extraction cartridges 11 ₁ to 11 described above
11 ₅ were individually housed and held the respective solid-phase extraction cartridge 11 ₁ to 11 ₅ and the tubular container body 4 integrally aforementioned
The cartridge holding cylinders 43E and 43F mounted inside the cartridge 3 are provided.

Here, one cartridge holding cylinder 43E
Is the solid-phase extraction cartridge 11 located at the upper end of FIG.
_It is equipped for ₁ and the other cartridge holding cylinder 43F
And are formed to be somewhat shorter in length. Also, the other cartridge holding barrel 43F is equipped individually to other solid-phase extraction cartridge 11 _{2-11 5,} and is equipped with is accommodated in the cylindrical container body 43 as described above. (See FIG. 8).

The one cartridge fixing body 46 provided on the mobile phase introduction side is provided in a state of being inserted into the upper end portion of the cylindrical container body 43 in FIG.

The one cartridge fixing body 46 is provided with the mobile phase introducing portion 13A at the center of the upper end portion in FIG. The mobile phase introducing portion 13A is configured similarly to the case of FIG. 1 described above, and the introduction guide hole 13Aa formed on the central axis of the cartridge fixing body 46 and the introduction guide hole 1
3Aa and a piping piece 13Ab screwed from the outside.

In this case, the solid-phase extraction cartridge 11 ₁ is connected to the _one cartridge fixing body 46 by connecting the first container main body 13 in the case of FIG.
Are connected in exactly the same state as the engaged state with respect to.

Further, the other cartridge fixing body 47 provided on the mobile phase sending side is provided so as to be vertically movable while being inserted in the lower end portion of the cylindrical container body 43 in FIG.

The other cartridge fixing body 47 is provided with a mobile phase sending portion 18A at the center of the lower end portion in FIG. The mobile phase delivery portion 18A is configured similarly to the case of FIG. 1 described above, and the delivery guide hole 18Aa formed on the central axis of the cartridge fixing body 47 and the delivery guide hole 1 are provided.
8Aa and a piping piece 18Ab screwed from the outside. In this case, the solid phase extraction cartridge 11 for the other cartridge fixing body 47
The connection of ₅ is performed in the same state as the engagement state with the sixth container body 18 in the case of FIG. 1 described above.

Here, the symbol S is the inner diameter of both ends of the cylindrical container body 43 and the above-mentioned one and the other cartridge fixing bodies 4.
6 shows a sealing mechanism for sealing between 6 and 6. Also, reference numeral 2
B and 2C show sealing O-rings that constitute a sealing mechanism for sealing the connection between the solid-phase extraction cartridges 11 _{1 to} 11 ₅ .

The first cap mechanism 44 described above is also used.
8 is formed in an inverted U-shaped cross-section with an open lower part in FIG. 8, a female screw portion is formed on the inner diameter side of the opening, and a male screw portion formed on the outer periphery of the upper end portion of the cylindrical container body 43 is screwed. It is supposed to be combined. This first cap mechanism 4
At the central portion of 4, the one cartridge fixing member 4 described above
A through hole 44a for projecting the mobile phase introducing portion 13A equipped in the No. 6 upward is formed. Reference numeral 44A indicates an annular elastic member, and reference numeral 44B indicates a seat. And
The first cap mechanism 44 is firmly screwed to the cylindrical container body 43 by the repulsive force of the annular elastic member 44A.

The above-described second cap mechanism 45 is formed in a U-shaped cross section, has an internal thread portion on the inner diameter side of its opening, and has a male thread portion formed on the outer periphery of the lower end portion of the cylindrical container body 43. It is designed to be screwed. A through hole 45a for allowing the lower end portion of the other cartridge fixing body 47 and the mobile phase sending portion 18A to project downward is formed in the central portion of the second cap mechanism 45. This through hole 45a portion The cartridge fixing body 47 described above is partially fixed and mounted. Reference numeral 47A indicates a brim portion for locking.

Then, by turning the second cap mechanism 45, the contact pressure between the solid phase extraction cartridges 11 _{1 to} 11 ₅ mounted in the cylindrical container body 43 is adjusted appropriately. Has become.

In this way as well, the operation and effect are almost the same as those of the embodiment of FIG. 1 described above, and in particular, the solid phase extraction inside is simply performed by removing the first and second cap mechanisms 44 and 45 at both ends. The cartridges 11 _{1 to} 11 ₅ can be easily taken out or stored, and thus workability can be further improved, and long screws or the like are not required, so that the cylindrical closed container 42 itself can be made smaller. It is possible to reduce the weight and the weight, and thus the portability is significantly improved.

In each of the above embodiments, the case where five solid-phase extraction cartridges are provided is illustrated, but the present invention is not limited to five solid-phase extraction cartridges.

[0088]

Since the present invention is constructed and functions as described above, according to this, in the invention according to claim 1,
Using an inexpensive solid phase extraction cartridge made of plastic, it is possible to extract the same components as in the case of a super expensive stainless steel column, and it is possible to simultaneously extract multiple types of components in a sample with one measurement. As a result, the analysis time of the components can be greatly shortened. In particular, simultaneous extraction of multiple components enables simultaneous extraction of new components, and repeated use of a cylindrical closed container. Since it is possible to significantly reduce the time and labor required for component extraction and the required cost in the conventional example, it is possible to greatly improve the reliability of the entire device in this respect, which is an excellent liquid chromatography for which it has not existed before. A column device can be provided.

Further, according to the invention described in claim 2, in addition to having the same operation and effect as the invention described in claim 1, the number and position (linking order) of the solid phase extraction cartridges can be grasped, so that the solid phase extraction cartridge is fixed. The phase extraction cartridge can be easily managed, and the component extraction work can be carried out more quickly and smoothly than the conventional one in this respect, and the component leakage from the connection part of each solid phase extraction cartridge can be effectively eliminated. You can

Furthermore, in the invention described in claim 3, in addition to the same effect as the invention described in claim 1 or 2, leakage of components from the connecting portion between a plurality of solid phase extraction cartridges is achieved. Can be eliminated more completely, which can further improve the reliability of the measurement technique and the device.

[Brief description of drawings]

FIG. 1 is a cross-sectional view showing a first embodiment of the present invention.

FIG. 2 is a block diagram showing an example of a liquid chromatograph incorporating the embodiment shown in FIG.

FIG. 3 is a sectional view showing a second embodiment of the present invention.

FIG. 4 is a partial cross-sectional view showing a modified example of the first container body in the second embodiment shown in FIG.

FIG. 5 is a view showing a modified example of the seal portion of the sixth container body in the second embodiment shown in FIG. 3, and FIG. 5 (A) shows an example in which two large and small annular seal members are combined. FIG. 5B is a partial sectional view showing the example in which a sealing O-ring is provided.

FIG. 6 is a view showing a modified example of the seal mechanism of the connecting portion between the solid phase extraction cartridges in the second embodiment shown in FIG. 3, and FIG. 6 (A) shows a case where two annular deformable seal members are combined. Partial sectional view showing an example, FIG. 6B is a partial sectional view showing an example in which a diamond-shaped annular deformable seal member and a sealing O-ring are combined, and FIG. 6C is a cylindrical outer peripheral surface. FIG. 6D is a partial cross-sectional view showing an example of a case where a deformable seal member having a mountain-shaped inclined surface is provided, and FIG. It is a partial cross-sectional view showing an example of.

FIG. 7 is a sectional view showing a third embodiment of the present invention.

FIG. 8 is a sectional view showing a fourth embodiment of the present invention.

FIG. 9 is a block diagram showing a liquid chromatograph incorporating a conventional example.

[Explanation of symbols]

2 Sealing mechanism 2A Cylindrical member 2B, 2C Sealing member 11 ₁ , 11 ₂ , 11 ₃ , 11 ₄ . 11 ₅ Solid Phase Extraction Cartridge 11a Mobile Phase Inlet 11b Mobile Phase Outlet 12, 22, 32, 42 Cylindrical Sealed Container 13, 14, 15, 16, _17, 18 Container Main Body 23, 24, 25, 26, 27 , 28 container body 33, 34, 35, 36, 37, 38 container body 43 tubular container body

Claims (3)

[Claims] 1. A cylindrical hermetic container equipped with a plurality of solid-phase extraction cartridges detachably connected in series, with the mobile phase inlet and the mobile phase outlet of each solid-phase extraction cartridge communicating with the outside. And a sealing mechanism for sealing the connection part to the outside of the solid-phase extraction cartridge in the vicinity of the connection part of each solid-phase extraction cartridge installed in the cylindrical closed container. A column device for liquid chromatography. 2. The column device for liquid chromatography according to claim 1, wherein the cylindrical closed container is divided into a plurality of container body portions for each of the solid phase extraction cartridges, and the plurality of divided containers are separated. A column device for liquid chromatography, wherein the main body parts are connected to each other while maintaining a sealed state. 3. A cylindrical member equipped with the sealing mechanism around a connecting portion of a plurality of solid phase extraction cartridges,
The column device for liquid chromatography according to claim 1 or 2, wherein the column member for liquid chromatography comprises a seal member provided between both ends of each cylindrical member and each solid phase extraction cartridge.