JPH0394158A - Chromatography device and forming device for component separating means - Google Patents

Abstract

PURPOSE:To execute a continuous separation in columns by providing a first substrate in which grooves of a mesh are formed and a second substrate which covers airtightly the grooves and fixed to become columns of a mesh, and forming a component separating means in the columns. CONSTITUTION:In grooves 11 in the direction as indicated with an arrow X of the mesh-like grooves 11 formed in a regular square, at least two kinds of component separating members 21 are formed, and the grooves 11 in the direction as indicated with an arrow Y are in an unprocessed state. Carrier gas is led into columns from the directions as indicated with arrows C1, C2 through a carrier gas distributing groove, and flows out in the directions as indicated with arrows D1, D2. In the case sample gas having components A, B is led into one point O of mesh-like columns, the sample gas advances at the same speed in the OY direction, but in the OX direction in which the separating members 21 are formed, a difference of a speed of flowing out is generated in accordance with the component, and it flows out from different outlets (points P, Q). Accordingly, by sensors provided in the vicinity of the tips of those outlets, the components A, B can be detected continuously, and by executing a waveform processing, concentration of the components A, B can be known by executing a waveform processing.

Description

[Detailed Description of the Invention] Field of Use in Industry 2〉 The present invention relates to the Chroma 1 to Craffy device, and the present invention relates to the Chroma 1 to Craffy device, which enables continuous separation measurement and has a longer service life by eliminating the need for a switching valve. Relating to a graphics device.

BACKGROUND ART A conventionally used gas chromatography apparatus (hereinafter simply referred to as gas chromatography), for example, has a configuration as shown in FIG. That is, the flow of the carrier gas and the sample gas is switched by a switching valve 1, and the sample gas carried by the carrier gas is passed through the column 2 through the switching valve 1 to be separated into components, and the components of the separated gas are separated. is measured by detector 3.

Problems to be Solved by the Invention In the above-mentioned conventional technology, measurements are basically made in a batch manner, and for process cask helmets, the sequence control is 1 cola, and the LIJ replacement valve is periodically replaced by 17J.

Furthermore, in conventional laboratory cassettes, sample fluid is injected manually using a microsyringe. However, when cascro systems become smaller and more micro in the future, those that use conventional switching valves will have problems in terms of switching valve performance (particularly leakage), lifespan, and miniaturization. In the case of using a syringe, there is a problem in that when the sampling amount is as small as n(1.p(l), the structure of the syringe has a limit.

The present invention has been developed in light of the above problems of the prior art, and aims to provide a chromatography apparatus that does not require a switching valve by providing a column with a continuous separation function.

A first configuration of the present invention for solving the second problem includes a first substrate in which a mesh groove is formed, and a mesh column that airtightly covers the groove. a second substrate fixed so that
at least two types of component separation means formed in a column in any specific direction of the mesh column; a carrier fluid introduction means for introducing a carrier fluid into one end of each of the mesh columns; The second structure is characterized by comprising a sample fluid introducing means for introducing the sample fluid into the column mentioned above from one point of the fluid introduction point. a second substrate fixed to the substrate so as to airtightly cover the well to form a mesh column; and at least two types of component separation means formed in columns in any specific direction of the mesh column. , a chromatography apparatus comprising a carrier fluid introduction means for introducing a carrier fluid into one end of each of the mesh columns, and a sample fluid introduction means for introducing a sample fluid into the column from a point on the carrier fluid introduction side, The component separation means is a first
In one direction of the substrate, a component separation means is applied by diagonal vapor deposition on both sides of the grooves of the mesh, and then a component separation means adhering to the surfaces other than the grooves of the mesh and the bottom of the bottom of the mesh is separated. It is characterized in that it is formed by a step of removing the means by anisotropic etching.

According to J. Kibo, a sample fluid containing multiple components that flows into a mesh column is carried forward by a carrier fluid that flows into the end of the column, but the components are not separated. Since the means are formed in any particular direction of the column, the sample fluid is delayed depending on its composition. As a result, only fluids with specific components are discharged at each outlet of the column. By placing sensors at the outlets of these columns, it is possible to continuously measure the components of different types of fluids.

Example Hereinafter, the present invention will be explained based on the drawings.

FIG. 1 is a perspective view showing an embodiment in which the present invention is applied to a gas chromatography apparatus. In Figure 1, 1
0 is a first substrate made of, for example, a Si wafer, and 11 is a fine groove formed in a lattice pattern on the surface of this substrate 10 by photolithography and etching technology (PA grooves are 500 in the vertical direction and 500 in the horizontal direction). 500 pieces), and the portion where the bowls 11 are formed has a square mesh shape as a whole. At least two types of component separating members are formed in the hot water in any specific direction (direction of the arrow X shown in the figure) among these water heaters 11. Reference numeral 12 denotes carrier gas distribution slides formed in the vicinity of two adjacent sides of the square-shaped mesh groove 11, and one end of each groove 11 communicates with the carrier waste distribution groove 2.

Reference numeral 13 denotes a mixed waste trapping groove formed on the opposite side of the carrier gas distribution groove 12, and the pond ends of each groove 11 are communicated with each other. 1
4 is a waste sensor formed in each groove 11;
The end portion of the groove 13 is disposed just before reaching the mixed gas trapping groove 13. Reference numeral 15 denotes an electronic circuit section that performs peak detection, waveform processing, calculation, etc., and is connected to the gas sensor 14 through a lead wire 16.

17 is an output terminal for taking out a signal from the electronic circuit section 15. Reference numeral 18 denotes a second substrate made of a Si wafer similar to the first substrate, and this second substrate 18 is bonded by a known anodic bonding method, etc.
1 to form a grid-like column. 19 is a carrier waste introduction hole communicating with the carrier waste distribution vortex 12 of the first substrate, and 20 is a sample gas introduction hole communicating with the corner of the grid-like column.

Figure 2 is an enlarged view of the mesh part of the device shown in Figure 1 (a).
and FIG. 7(b) is an enlarged view of part A of the groove. In FIG. 2, a component separating member 21 is formed in the groove in the direction of arrow X, as shown in the cross section B-B in FIG. It is said that In addition,
The component separating member 21 is formed by filling or coating a filler or treating the surface of the groove.

2, the carrier waste is introduced into each column from the directions of arrows C I and C through the carrier gas distribution groove 12, and flows out in the directions indicated by arrows DI and D2.

Figure 3 shows the movement of gas when a sample blade containing components A and B is introduced into one point (0) of a mesh column through which carrier gas is flowing (here, component B is delayed in the component separation member compared to component A).

In other words, the sample gas flowing into the mesh column advances at the same speed in the OY direction (unprocessed direction), or at least two types of component separation members are formed in the OX column.
Similar to conventional separation columns, there are differences in the outflow velocity depending on the component, resulting in different exits (point 1).
, Q). Therefore, if a sensor is provided near the tips of these outlets, components A and B can be detected continuously, and the concentration of each component can be determined by performing waveform processing.

FIG. 4 shows, for example, the number of vortices is 500×500, and shows the calculation result of the extent to which the debris flowing from point O spreads in a direction perpendicular to the traveling direction.

Each streamline connects the positions of 5%, 50%, and 95% of the peak value in the outflow direction.

FIG. 5 shows the spread of sample cassettes with respect to the number of grooves, with the highest value being normalized to 1.

With the above configuration, components contained in the sample gas flow out from different outlets, eliminating the need for a switching valve and allowing continuous measurement.

Furthermore, there is no malfunction caused by using a switching valve.

8 FIGS. 6 and 7 are process diagrams and work flows showing the process of forming component separation means only in arbitrary specific directions of the circular surfaces on both sides of the mesh groove, according to the second embodiment of the present invention. . In FIG. 6(a), the vertical lines of the mesh grooves 11 formed on the first substrate 10 are aligned in one horizontal direction to the base of the 3-dimensional surface of the J-law (for example, the bright surface 1. The component separating member is deposited diagonally from above at an angle such that the base of the rfii l l b is visible when viewed from 1a (FIG. 7(a)).

The component separating member is deposited thickly on both open faces of the groove 11, and thinly on the faces other than the groove 11 and the bottom of the groove 11. Next, the component separation member that has adhered to the surface other than the groove 11 and the bottom surface of the groove 11 is removed, but the component separation member that has adhered to the surface other than the groove 11 and the bottom surface of the groove 11 is adhered to both open surfaces of the groove 11. The direction of adhesion is different for the component separation member. Therefore, by performing directional anisotropic etching (FIG. 7(b)), the sixth
As shown in Figure (b), component separation members 21 are formed only on both vertically and horizontally open faces. (In the figure, component separation members 21 are formed on both sides of the horizontal groove. 〉 In the above embodiment, the mesh was shaped like a lattice, but for example, as shown in FIG. By forming members, it is possible to obtain the same effect as a grid-like one, and the column shape (. It can be changed arbitrarily depending on the state of component separation.

In addition, in the above-mentioned grid-shaped embodiment, component separating members were formed in the grooves in one direction and no treatment was made in the other direction, but it is also possible to form component separating members in different scales. It is possible. By using such different types of component separation members, it is not only possible to separate a wide variety of components, but also to further improve the separation performance of this column. This means that, for example, in the hexagonal shape shown in Figure 8,
Different types of component separating members may be formed in the (a) direction and (c) and (ii) direction.

In this embodiment, the case where the present invention is applied to gas chromatography has been described, but it is also possible to apply it to a liquid chromatography apparatus.

In addition, in this example, we have shown an example of application to microstructures, or we have used another material (for example, metal or plastic) as a substrate, formed columns by machining, etc., and calculated the total area of the mesh by several steps. It is also possible to use it as a separation device for separating the components of a liquid containing a plurality of components with a size of 10 C rivers to several rivers 1/direction.

Effects of the Invention> As described above in detail with the embodiments, according to the present invention, a switching valve is not necessary and continuous measurement is possible. Furthermore, since no switching valve is used, a chromatography apparatus with fewer failures can be realized.

[Brief explanation of drawings]

FIG. 1 is a W4 perspective view showing an embodiment of the chromatography apparatus of the present invention, and FIGS. 2(a) and (b) are enlarged views of the mesh portion and the groove portion of the apparatus shown in FIG. Figure 3 is a diagram showing the principle of component separation of the apparatus shown in Figure 1, Figure 4 is a diagram showing the principle of component separation of the apparatus shown in Figure 1.
The figure shows the distribution state of the peak of component 11 in the column, Figure 5 shows the normalized spread of sample gas with respect to the number of grooves, and Figures 6 and 7 show the second aspect of the present invention. A process diagram and a work flow showing a process of forming a component separation means only in an arbitrary specific direction of a double-sided measurement surface of a mesh groove showing an embodiment, FIG. 8 is a diagram showing another example of a column, FIG. 9 is a diagram showing the principle of a conventional gas chromatography apparatus. DESCRIPTION OF SYMBOLS 10... First substrate, 11... Groove, 12... Carrier gas distribution groove, 13... Mixed gas capture groove, 14...
・Sensor, 15...Electronic circuit section, 16...Lead wire, 17...Output terminal, 18...Second board, one.
... Carrier gas introduction hole, 20 ... Sample gas introduction hole, 21 ... Component separation member. 12 5th Figure 0 20 30 40 50

Claims (1)

Scope of Claims: (1) A first substrate on which a mesh groove is formed, a second substrate that is fixed to form a mesh column so as to airtightly cover the groove, and a second substrate formed with a mesh column; at least two types of component separation means formed in a column in any specific direction; a carrier fluid introduction means for introducing a carrier fluid into one end of each of the mesh columns; A chromatography apparatus comprising a sample fluid introducing means for introducing a sample fluid into the chromatography apparatus. (2) The chromatography according to claim 1, characterized in that at least two types of component separation means formed in the column in any particular direction of the mesh column are formed on both sides of the mesh groove. Device. (3) A first substrate in which a mesh groove is formed, a second substrate that is fixed to the mesh column so as to airtightly cover the groove, and a column in any specific direction of the mesh column. at least two types of component separation means formed therein, a carrier fluid introduction means for introducing a carrier fluid into one end of each of the mesh columns, and a sample fluid introduced into the column from a point on the carrier fluid introduction side. A method for forming a component separating means, in a chromatography apparatus comprising a sample fluid introducing means, wherein the component separating means is formed by the following steps. (1) A step of applying a component separation means to the side surfaces on both sides of the mesh grooves by an oblique vapor deposition method in any one direction of the first substrate on which the mesh grooves are formed. (2) A step of removing the component separation means attached to the surfaces other than the mesh grooves and the bottom surfaces of the mesh grooves by anisotropic etching.