WO2006025557A1

WO2006025557A1 - Device to purify and concentrate compound and method for purifying and concentrating compound using the device

Info

Publication number: WO2006025557A1
Application number: PCT/JP2005/016175
Authority: WO
Inventors: Yoshio Fujiwara; Akiko Shinoda; Yoshihiro Ohki
Original assignee: Showa Denko KK
Current assignee: Resonac Holdings Corp
Priority date: 2004-08-31
Filing date: 2005-08-30
Publication date: 2006-03-09
Anticipated expiration: 2007-02-28

Abstract

The present invention relates to a compound purification-concentration device, which has a packing material for purifying and concentrating a compound and a fluid permeating plate for holding the packing material at each end surface of the packing material in a container having an inflow port and an outflow port for a fluid, being characterized by having a space portion at an outer surface of the fluidpermeatingplate at each end surface, and a purification-concentration method using the device. In the present invention, the device is designed such that when the fluid is a gas and is flown at a flow rate of 6 to 12 L/min, a linear velocity of the gas which passes through a side face of an imaginary column formed by a plane which is vertically dropped from a peripheral line of the inflow port or the outflow port of the fluid to the surface of the fluid permeating plate is to be 30 m/sec or less. The compound purification-concentration device of the present invention is characterized in that, while maintaining a high capacity of purifying and separating a compound, pressure to be generated at the time of gas-passing or liquid-passing is relatively low and a clogging less occurs even in a case of a sample having many suspended solids.

Description

DESCRIPTION

DEVICE TO PURIFYAND CONCENTRATE COMPOUNDAND METHOD FOR PURIFYING AND CONCENTRATING COMPOUND USING THE DEVICE

CROSS-REFERENCE TO THE RELATED APPLICATIONS

This is an application filed pursuant to 35 U.S.C. Section

111 (a) with claiming the benefit of U.S. Provisional application

Serial No. 60/607, 598 filed September 8, 2004 under the provision of 35 U.S.C. Section 111 (b) , pursuant to 35 U.S.C. Section

119(e) (1) .

TECHNICAL FIELD

The present invention relates to a device for purifying and/or concentrating a compound (in Claims and Specification of the present invention, "purifying and/or concentrating" is simply denoted as "purifying and concentrating") , and a method for purifying and concentrating the compound using the same.

BACKGROUND ART

Conventionally, a liquid absorption method for extracting a sample from a gas, and a liquid-liquid extraction method for extracting a sample from a liquid have been used in many cases. However, there were such problems that the methods required a complicated operation, a long period of time and experience and consumed a large amount of a solvent. On the other hand, a solid phase extraction method which has recently been adopted in many cases has characteristics such that an operation is simple, performed in a short period of time and an amount of the solvent to be used is small. For this reason, the solid phase extraction method is extremely advantageous when many samples are required to be collected in a short period of time, and also can easily be automated. A background in which the solid phase extraction method has rapidly been expanded in recent years can be accounted for by that porous particles which are excellent in an adsorption-desorption property have been developed and these porous particles have been provided in a market from a plurality of manufacturers as adsorbents for the solid phase extraction. As for commercially available adsorbents for the solid phase extraction, there are various shapes of articles such as a silica gel particle into which a functional group is introduced, apolymer particle such as a styrene-divinyl benzene copolymer, a carbonaceous particle such as activated carbon or carbon graphite and further, in recent years, activated carbon fiber prepared by sintering various types of synthetic fibers and a subsequent activating treatment or a rod-like porous continuous body (monolith) formed by polymerization in a column (bulk polymerization in the presence of a diluent) . An appropriate article can be selected in accordance with applications. In recent years, in regard to chemical substances which have remarkably been increased in types and amount, there is a growing demand for figuring out conditions of environmental pollutions thereof, and then it has become necessary to detect thinner components in a trace amount. Along with the needs, quantities of samples such as air and environmental water to be subjected to analysis have been increased and then, since the analysis involves a long period of time, it is required not only to enhance performance of a compound separation device but also to develop a rapid measurement method. For enhancing the separation performance of the compound separation device, many methods have been proposed so far. For example, a specific structure for effectively utilizing an entire area of a packing material has been proposed (JP-U No. 62-53342) . However, there has not been a proposal from the viewpoint of a rapid treatment. Further, in a method which aimed for enhancing a packing density or decreasing a number average diameter of the packing material or the like, improvement of purification-separation performance can be expected along with an increase of a surface area of the packing material; however, clogging is generatedbyaminute impurity solid (for example, dust or a suspended solids (ss) in liquid) and the like contained in a fluid, so it may give rise to a need of frequent change of separation devices in the middle of a pre-treatment, or, when the liquid is allowed to pass at a high rate, a pressure load to a column or an apparatus has become large and a treatment speed tends to be limited. Therefore, there have not been methods which fully satisfy the request for a rapid treatment. In fibrous packing materials or monolith packing materials, a low pressure resistance at the time of liquid-passing is one of the characteristics. However, in conventional separation devices, resistance arises from structural features at the time of fluid-passing, and therefore there has not been a device which isabletomakeuseofthecharacteristicsofthesepackingmaterials up to a satisfactory extent.

DISCLOSURE OF THE INVENTION

The onlyway to effectively adsorb an infinitesimal quantity of a chemical substance present in gas or liquid by a disk or a column filled with silica gel particles, polymer particles such as styrene-divinyl benzene copolymers, activated carbon, carbon graphite or the like, was to increase a packing density by allowing a packing material to be smaller in size so as to make a gap between the particles as small as possible, or to increase the amount of packing materials. However, in performing such measure as described above, since a pressure loss caused during passing gas or liquid becomes large, a problem arises such that a passing rate can not be increased, which leads to a long period of time required for passing a large amount of gas or liquid. Further, in a case in which there is a large amount of suspended solids such as microorganisms in the gas or liquid, a serious problem of clogging tends to take place in the middle of passing. On the other hand, when a particle diameter of the packing material or a diameter of the fiber is allowed to be larger or an amount of the packing material is decreased in order to alleviate the above-described problems, adsorbing efficiency is decreased and a satisfactory result can not be obtained.

The present invention has been achieved in the face of such circumstances. An object of the invention is toprovide a compound concentration device which is characterized in that, while maintainingahighcapacityofpurifyingandseparatinga compound, pressure to be generated at the time of gas-passing or liquid-passing is relatively low and a clogging less occurs even in a case of a sample having many suspended solids; and a purification-concentration method using the device.

The present inventors have exerted intensive studies on a methodforproducinga compoundpurification-concentrationdevice which is characterized in that, while maintaining a high capacity of purifying and separating a compound, a pressure loss to be generated at the time of gas-passing or liquid-passing is relatively low and a clogging less occurs even in a case of a sample having many suspended solids. As a result, the present inventors have found out that the object can be attained by not improving the packing material but improving a structure of the compound concentrationdevice, totherebyaccomplishthepresent invention.

That is, the present invention relates to a compound purification-concentration device and a method for purifying and concentrating a compound as follows :

1. Acompoundpurification-concentrationdevice, whichhas a packing material for purifying and concentrating a compound and a fluid permeating plate for holding the packing material at each end surface of the packingmaterial in a container having an inflow port and an outflow port for a fluid, being characterizedby having a space portion at an outer surface of the fluid permeating plate at each end surface of the packing material.

2. The compound purification-concentration device as described in 1 above, comprising a projected structure for holding the fluidpermeatingplate on an inner side surface of the container at the outer surface side of at least one fluid permeating plate.

3. The compound purification-concentration device¹ as described in 1 or 2 above, wherein an inner wall of the container at the outer surface side of at least one fluid permeating plate has a tapered structure.

4. The compound purification-concentration device as described in any one of 1 to 3 above, wherein a material which does not affect the purification-concentration of the compound is packed in the space portion.

5. The compound purification-concentration device as described in 4 above, wherein the material which does not affect the purification-concentration of the compound comprises one or moremembers selectedfromthegroupconsistingofaglassparticle, aglass fiber, aquartzparticle, aquartz fiber, aceramicparticle, ametallicparticle, ametallic fiber, apolymerparticle, apolymer fiber, gravel and sintered articles thereof.

6. The compound purification-concentration device as described in any one of 1 to 3 above, comprising a groove-like structure at the outer surface side of at least one fluidpermeating plate.

7. The compound purification-concentration device as describedin 6 above, whereinthe groove-like structure isprovided on an inner wall of the container. 8. The compound purification-concentration device as described in 1 or 4 above, wherein a volume of the space portion at one side is 0.2 to 50% of an entire volume, while a total volume of the space portions at both sides is 0.5 to 50% of an entire volume. 9. The compound purification-concentration device as described in any one of 1 to 8 above, wherein the packing material is a monolith (rod-like porous continuous body) or a fiber.

10. The compound purification-concentration device as described in any one of 1 to 8 above, wherein the packing material is in a spherical form, crushed formor amorphous grainy formhaving an average particle diameter of 5 μm or more.

11. The compound purification-concentration device as describedin 1, 4 or 10 above, whereinthepackingmaterialcomprises a material which undergoes change in volume by coming in contact with the fluid.

12. The compound purification-concentration device as describedin 11 above, wherein the volume change rate of the packing material is 0.5 to 50%.

13. The compound purification-concentration device as described in any one of 1 to 12 above, being in a form of a cartridge or a column for solid extraction.

14. The compound purification-concentration device as described in any one of 1 to 13 above, wherein one of the inflow port and the outflow port has a male structure and the other has a female structure capableofbeing coupledwiththemale structure.

15. The compound purification-concentration device as described in any one of 1 to 14 above, being designed such that when the fluid is a gas and is flown at a flow rate of 6 to 12 L/min, a linear velocity of the gas which passes through a side face of an imaginary column formed by a plane which is vertically dropped from a peripheral line of the inflow port or the outflow port of the fluid to the surface of the fluid permeating plate is to be 30 m/sec or less.

16. A method for purifying and concentrating a compound contained in a fluid, being characterized by using the compound purification-concentration device as described in any one of 1 to 15 above.

17. The method for purifying and concentrating a compound as described in 16 above, wherein the compound comprises one or moremembers selectedfromthe groupconsistingofanenvironmental pollutant, dioxins, endocrine disturbing chemicals, agricultural chemicals, a surfactant, abiotoxin, a natural medicine, a natural coloring agent, a natural fragrance and a natural seasoning.

18. The method for purifying and concentrating a compound as described in 16 above, wherein the fluid containing the compound is in the form of liquid and/or gas.

19. The method for purifying and concentrating a compound as described in 18 above, wherein the liquid is selected from among an environmental water, a biological fluid, a separated liquid, an extracted liquid and an absorbed liquid. 20. The method for purifying and concentrating a compound as described in 18 above, wherein the gas is selected from among an atmospheric air, an indoor air, a separated gas and an extracted gas. 21. A method for purifying and concentrating a compound inagas sample, whereinthe gas sample is flownbyusingthe compound purification-concentration device as described in any one of 1 to 15 above at a flow rate of 6 to 12 L/min such that a linear velocity is to be 30 m/sec or less when the gas passes through a side face of an imaginary column formed by a plane which is vertically dropped from a peripheral line of the inflow port or the outflowport of the fluid to the surface of the fluidpermeating plate.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic diagram of a compound purification-concentration device having a tapered structure which is an example of the compound purification-concentration device according to the present invention. FIG. 2 is a schematic diagram of the compound purification-concentration device of Comparative Examples.

FIG. 3 is a side view (A) and a plan view (B) schematically showing a compound purification-concentration device having a groove-like structure which is an example of the compound purification-concentration device according to the present invention.

FIG. 4 is an explanatory diagram of an imaginary column.

MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention is described in detail with reference to the accompanying drawings.

A compound purification-concentration device according to the present invention, as a schematic diagram of an example is shown in FIG. 1, which contains, inside a container (1) having an inflow port (5) and an outflow port (6) of a fluid, a packing material (4) for purifying or concentrating a compound to be measured or a useful compound contained in the fluid and fluid permeating plates (3a, 3b) for holding the packing material at both end surfaces of the packing material, is characterized in that space portions (7a, 7b) are provided at outer surface sides of the both fluid permeating plates (3a, 3b) , respectively.

The fluid permeating plates (3a, 3b) which have permeation pores (not shown) all over the plates are set so as that the fluid can be dispersed all over the packing material (4) and also the packing material (4) is prevented from being leaked from inside the container (1) . As for the fluidpermeatingplate, for example, an article having a thickness of about 0.5 to about 3 mm formed by sintering polyethylene particles or a filter made of paper or glass fiber can be used. For allowing the fluid to be dispersed all over the packing material after passing through the fluid permeatingplate, it is necessarytoprovide areas (spaceportions) (7a, 7b) through which the fluid easily passes to be dispersed all over the fluid permeating plate not only at the outer surface side of the fluid permeating plate at an inlet side but also at the outer surface side of the fluid permeating plate at an outlet side. Further, byproviding the space portions (7a, 7b), an effect of alleviating a pressure loss which is increased along with the increase of a fluid flow rate can be obtained. Further, since a solid content in the fluid can be dispersed all over the fluid permeating plate, an effect of alleviating generation of clogging can be obtained.

For retaining the space portions, projected structures may be provided on an inside surface of the container at the outer surface side of at least one fluidpermeatingplate. Theprojected structures may be provided on the entire circumference or a part of the circumference so longas it holds stablythe fluidpermeating plates. By the projected structures, the fluid permeating plate can easily be held.

Further, one method for providing the space portions (7a, 7b) is a method to provide a tapered structure (2) on an inside wall of the container at the outer surface side of the fluid permeating plate.

Byproviding the tapered structure (2), the fluidpermeating plate can easily be fixed in a state of having a space portion. A taper angle (θ) of the tapered structure is preferably 5 to 85°. When the angle is unduly small (when θ is unduly large) , by a force to be put on the fluid permeating plate when a fluid flow rate is increased or the packing material is expanded along with the fluid-passing, the fluid permeating plate is moved and the space portionis narrowed, orthepackingmaterialmayleakbydeformation or inclination of the fluid permeating plate. On the other hand, when the taper angle is unduly large (when θ is unduly small) , the space portion becomes insufficient and then, when the fluid flow rate is increased, a large resistance arises or clogging by the solid content in the fluid is easily generated.

Further, there is another method in which a material which does not affect the purification-concentration of the compound is packed at the outer sides of the fluid permeating plates (3a, 3b) . Such materials are, for example, glass, quartz, ceramics, metals and polymers. Shapes thereof are not particularly limited and include a particle shape, a fiber shape, a sintered shape, a non-woven shape, but it is necessary that a surface structure thereof does not affect the intended purification-concentration of the compound to a great extent. Further, when a particle diameter, a fiber diameter or void structure size of the material is unduly large, a uniformdispersion to the fluidpermeatingplate is hindered, which is not favorable; whereas, when it is unduly small, the material itself obstructs the flow of the fluid, which is not favorable. Further, still another method is a method to provide a groove-like structure on the outer sides of the fluid permeating plate. The shape of the groove is not particularly limited so long as it forms a structure such that the fluid is allowed to be scattered all over the fluid permeating plate. An unduly complicated structure generates a large pressure loss as the fluid flow rate is increased, which is not favorable.

As for the groove-like structure, as a side view and a plan view are shown in FIGS. 3(A) and 3(B), a groove-like structure (9) is preferred wherein projected structures (8) extend radially from the centers of an inflow port (5) and an outflow port (6) ofthe fluidto thewall. The groove-like structuremaybeprovided on the fluid permeating plate or an inner wall of the container. Further, aseparatelyformedarticlehavingagroove-likestructure may be provided. Width of the groove can be changed depending on a size of the container or a number of grooves, for example, the width of one groove can be defined as 33.3% or less of a length of a circumference of a concentric circle to the point and a total width of the all grooves can be defined as 50 to 99% of a length of a circumference of a concentric circle to the point. Further, depth of the groove can be changed depending on a size of the container and, for example, it can be defined as 0.2 to 50% of a length of from the base of the inflow port to the base of the outflow port. When the width is unduly large, strength for supporting the fluid permeating plate becomes weak, which is not favorable; whereas, when it is unduly small, a cross-sectional area which the fluid passes through is decreased, which is not favorable. Further, when the depth of the groove is unduly large, a size of the container itselfbecomes larger than necessary, which isnot favorable; whereas, when itisundulysmall, the spaceportion becomes narrow, which is not favorable.

For these reasons as mentioned above, a volume of the space portion at one side is preferably in the range of 0.2 to 50% of an entire volume and a total volume of the space portions at both sides is preferably in the range of 0.5 to 50% of an entire volume. According to the present invention, when a gas is flown at a flow rate of 6 to 12 L/min which is two to four times faster than the conventional flow rate in a cartridge having a column size as described in Example 1, as shown in FIG.4, it is preferable to define a cross-sectional area such that a linear velocity of the gas is to be 30 m/sec or less, when passing through a side face (π-d-h, wherein d represents a diameter of an inflow port or an outflow port; h represents a height of an imaginary column in a space portion) of an imaginary column (10) to be formed by a plane which is vertically dropped from a peripheral line of an inflow port or an outflow port of the fluid to a surface of the fluid permeating plate, and such that a maximum flow rate (linear velocity) of the fluid dose not exceed 30 m/sec in any part of the space. When the maximum flow rate exceeds 30 m/sec, a pressure loss becomes large, and accordingly, a flow rate per hour to be treated lowers. Further, as shown in FIG. 3, when a groove-like structure is providedat the outer surface side of fluidpermeating plate, it is preferable to design such that a flow rate when the fluid passes at a narrowest place is set to 15 m/sec or less. A linear velocity of the fluid which passes through the side face of the imaginary column (10) varies depending on a flow rate of the fluid passing through an entire column. Therefore, at the timeofdesigning, thepassingspeedatthesidefaceoftheimaginary column is arranged to be 30 m/sec or less at a flow rate conceivable in an actual use. Meanwhile, a lower limit of the passing speed at the side face of the imaginary column is not particularly defined so long as the fluid containing the compound can flow without anypractical problem. Furthermore, it is preferable that the projected structure (8) for imparting an open space is in contact with the fluid permeating plate in a smaller area because the pressure loss is reduced.

The packing materials to be used in the present invention range widely from a silica gel type to an organic polymer type, alumina, zeolite, hydroxyapatite, activated carbon, silicon carbide and the like. Shapes thereof have a wide variety such as a porous spherical particle, a crushed particle, fiber and a rod-like porous continuous body (monolith) .

One of characteristics of the fiber or monolith is a small pressurelossatthetimeofliquid-passing. Onecantakeadvantage of the characteristic by using the fiber or monolith in the purification-concentration device according to the present invention, since the resistance at the time of liquid-passing attributable to the structure is decreased and therefore liquid-passing is not obstructed. In a case of the spherical particle or the crushed particle, in order to improve capacity to separate a compound, an average particle diameter is allowed to be decreased; however, when the average particle diameter comes to be 5 μm or less, the resistance at the time of liquid-passing increases regardless of the structure of the purification-concentration device, which is not preferable. Further, in a case of a packing material such as a polymer type, for example, polystyrene or a poly(meth)acrylate, the particle thereof is expanded when it comes into contact with the fluid, which accompanies volume change of the packing material. On this occasion, the fluid permeating plate is push-expanded at the time of liquid-passing. In the purification-concentration device according to the invention, since the space portions are constitutionally provided at the outer sides of the fluid permeatingplates, the fluidpermeatingplate is tightlyin contact with the inner wall of the container and, accordingly, the passing property of the liquid is not impaired. Therefore, it is far more effective to use the purification-concentration device according to the invention in a case of the packing material having volume change of 0.5 to 50%. Forms of the compound concentration devices according to the invention are not particularly limited and representative examples include a column, a cartridge, a disk, a filter, a plate and a capillary.

The compounds to be purified and concentrated (separated) according to the invention include one or more compounds selected from the group consisting of compounds present in environmental water, a bottom sediment or atmospheric air such as dioxins, endocrine disturbing chemicals, a biotoxin and an agricultural chemical; compounds present in a biological fluid or a tissue of an animal or a plant such as a medicine, an agricultural chemical, a surfactant, a hormone, a neurotransmitter, a vitamin and a metabolite thereof; and compounds contained in a natural product such as a natural medicine, a natural coloring agent, a natural fragrance and a natural seasoning. Further, as for liquids or gases containing compounds to be separated, examples are environmental water such as rainwater, streamwater, lakewater, cleanwater, sewage, industrial effluent and sea water; a biological fluid such as urine and blood, or a separated liquid or an extracted liquid thereof; an extracted liquid from a tissue of a plant or an animal; and an environmental atmospheric air such as an incinerator flue gas, emission gases from various types of production facilities, an indoor air, an automobile exhaust gas, an atmospheric air collected above an arterial highway or an absorbed liquid prepared by allowing such air or gas as described above to be passed through a liquid.

Themethodforpurifyingandconcentratingthecompoundusing the compound purification-concentration device according to the invention is not particularly limited, so long as a main object thereof is, by allowing a liquid or a gas containing a compound (a material to be measured or a useful material) to pass through, to perform purification by adsorbing a material which obstructs a measurement of the compound or to perform purification and/or concentration after a compound is once adsorbed by the packing material, byelutingthecompoundwithasolvent. Atypicalexample is capturing andconcentrating an environmental pollutantbyusing a cartridge for solid phase extraction.

In a case of purifying and concentrating a compound by using the cartridge for the solidphase extraction, a cartridge prepared by filling a packing material and the fluid permeating plates for holding the packing material in a syringe type container made of polyethylene or the like can be used. In a case of the syringe type container, a specified device for coupling is required. In recent years, although many cartridges capable of being coupled without using such specified device have been used, there are many cases in which a volume of a filling portion including fluid permeatingplates is limitedin suchcartridges duetoarestriction on designing. Further, as described above, when volume change of the packing material occurs, for example, by the expansion of the packing material by coming into contact with the fluid, the fluid permeating plate is strongly pushed against the inner wall of the container andcomes tightly in contact therewith, to thereby markedly increase resistance at the time of passing through the fluid. Therefore, as a cartridge for the solid phase extraction having a structure capable of being coupled without a specified device, the cartridge according to the invention is extremely useful.

EXAMPLES

Hereinafter, the present invention is described in more detail with reference to examples, however, the present invention is not limited by the following Examples.

Example 1

In a cartridge having an inner diameter of about 12 mm, about 300 mg of polystyrene particles having a diameter of 500 to 700 μm was filled being sandwiched and held by two fluid permeating plates prepared by sintering polyethylene particles. At each of the outer surface sides of the both fluid permeating plates, as shown in FIG. 1, a tapered structure was provided such that a space having a height of about 2 mm at a central portion is formed. In this case, the inner diameter of an inflow port (outflow port) was 2 mm and a side face area of an imaginary column formed between the fluid permeating plate came to be 2 x 2 x π mm²=1.26 x ICT⁵ m². The cartridge was connected with a vacuum pump and aeration wasperformedbya suckingmethod, andsubsequently, adifferential pressure between an upstream side and a downstream side of the cartridge was measured while changing the aeration rate. As a result, when the aeration was performed at an aeration rate of 6 L/min which was faster than an ordinary rate (2.8 L/min) , the aeration linear velocity at the side face of the imaginary column was 6 L/min / 60 / (1.26 x 10^"5) m² / 1000 = 8.0 m/sec, and when the aeration was performed at a differential pressure of the cartridge of about 60 hPa and at an aeration rate of 8 L/m, the aeration linear velocity at the side face of the imaginary column was 10.6 m/sec and the differential pressure of the cartridge was about 90 hPa.

Example 2

In the cartridge (1) having an inner diameter (W) of about 12 mm, as shown in FIG. 3, about 300 mg of polystyrene particles having a diameter of 500 to 700 μm was filled being sandwiched and held by two fluid permeating plates prepared by sintering polyethylene particles. At each of the outer surface sides of the both fluid permeating plates, projections (8) (L = 3 mm) were provided such that a space having a height (h) of about 1.5 mm at a central portion was formed, to construct a radiant fan-shaped groove-like structure (9) . In this case, an inner diameter (d) of an inflow port (5) (outflow port (6) ) was 2 mm and a side surface area (d-h-π) of an imaginary column formed between the fluid permeating plate came to be 2 x 1.5 x π mm² = 0.94 x 10^~5 m². The cartridge was connected with a vacuum pump and aeration was performed by a sucking method, and subsequently, a differential pressure between an upstream side and a downstream side of the cartridge was measured while changing the aeration rate. As a result, at an aeration rate of 6 L/min and 8 L/min, an aeration linear velocity at the side face of the imaginary column was 10.6 m/sec and 14.2 m/sec, the differential pressure of the cartridge was about 65 hPa and about 100 hPa respectively.

Comparative Example 1

A cartridge (filled with about 300 mg of polystyrene particles having a diameter of 500 to 700 μm) , as schematically shown in FIG.2, having a same diameter as in Example 1 but without having a tapered structure was prepared. Byusing this cartridge, a test was performed in the same way. When aeration was performed at an aeration rate of 3 L/min, a differential pressure of the cartridge was about 108 hPa. A measurement was unable to be performed at a higher flow rate than the above described rate, due to being out of a practical measuring range.

Comparative Example 2

A cartridge (filled with about 300 mg of polystyrene particles having a diameter of 500 to 700 μm) having a same diameter as in Example 1 and having a structure forming a space having a height of about 0.5 mm at a central portion at each of the outer surface sides of the both fluid permeating plates was prepared. In this case, an inner diameter of an inflow port (outflow port) was 2 mm and a side surface area of an imaginary column formed between the fluid permeating plate came to be 2 x 0.5 x π mm²=0.31 x 10^"5 m². By using this cartridge, a test was performed in the same way. When aeration was performed at an aeration rate of 6 L/min, an aeration linear velocityat the side face of the imaginary column was 31.8 m/sec and a differential pressure of the cartridge was about 190 hPa. A measurement was unable to be performed at a higher flow rate than the above described rate, due to a large pressure loss.

Example 3

In a cartridge of the same type as used in Example 1, about 300 mg of polystyrene particles having a diameter of 50 to 90 μm was filledbeing sandwichedandheldby two fluidpermeatingplates produced by sintering polyethylene particles. The cartridge was connected with a metering pump and then purified water was allowed to pass by a pressure method, and thereafter, a pressure at an upstream side of the cartridge was measured while changing liquid-passing rate. As a result, the pressure at the upstream side of the cartridge was about 85 hPa, about 160 hPa and about 330 hPa when a liquid was allowed to pass at a liquid-passing rate of 10 mL/min, 20 mL/min and 40 mL/min, respectively.

Comparative Example 3

In a cartridge of the same type as used in Comparative Example 1, about 300 mg of polystyrene particles having a diameter of 50 to 90 μmwas filledbeing sandwichedandheldbytwo fluidpermeating plates produced by sintering polyethylene particles. By using this cartridge, a same test as in Example 2 was performed. As a result, the pressure at the upstream side of the cartridge was about 160 hPa, about 240 hPa and about 420 hPa when a liquid was allowed to pass at a liquid-passing rate of 10 mL/min, 20 mL/min and 40 mL/min, respectively. Example 4

By using the cartridge used in Example 3, an addition-recovery test of an agricultural chemical bendiocarb was performed.

Procedures: Two cartridges were coupled and subjected to a pre-treatment by allowing 10 mL of acetone/ethyl acetate (1:1) , 10 mL of methanol and 10 mL of purified water to pass therethrough. A test liquid (1 L of purified water) which was added with 50 μL ofbendiocarbinmethanolwhichwas adjustedtohavea concentration of 300 ppm was allowed to pass therethrough at each rate of 10 mL/min, 30 mL/min and 50 mL/min. From each cartridge which has been subjected to the liquid-passing, bendiocarb was eluted by using 10 mL of acetone/ethyl acetate (1:1) and the resultant solution was concentrated into 0.5 mL by gently blowing a nitrogen gas, and then made up to be 3 mL with acetonitrile, and thereafter subjectedtoanalysisbyan HPLC (UV: 254 nm) todetermine a recovery rate.

Results: At any liquid-passing rate, the recovery rate was 94 to 98%.

Comparative Example 4

By using the cartridge which was used in Comparative Example 3, anaddition-recoverytestofanagricultural chemicalbendiocarb was performed.

Procedures: Same as in Example 3.

Results: When the liquid-passing rates were 10 mL/min and 30 mL/min, recovery rates were both 94%; whereas, when the liquid-passing rate was 50 mL/min, liquid-passing was unable to be performed due to a large pressure loss. Example 5

By using the cartridge which was used in Example 3, a liquid-passing property test of stream water was performed. Procedures: Two cartridges were coupled and stream water of River T in Kanagawa Prefecture (collected in May) was sucked in and allowed to pass through the cartridge by means of a vacuum pump at -0.07 to 0.075 MPa and, then, a passing-liquid rate was measured with time. Results: The liquid-passing rate immediately after the liquid-passingwas startedwas about 25 mL/min and it was decreased to 20 mL/min in two minutes; however, even after one liter was allowed to be passed, the liquid-passing rate was least changed, to thereby maintain 18 mL/min or more.

Comparative Example 5

By using the cartridge which was used in Comparative Example

3, a liquid-passing property test of stream water was performed.

Procedures: Same as in Example 5. Results as follows: The liquid-passing rate immediately after the liquid-passing was started was about 10 mL/min.

Thereafter, the liquid-passing rate soon started to decrease and after 500 mLwas passedthrough the cartridge, the liquidwas hardly passed due to clogging.

INDUSTRIAL APPLICABILITY

The compound concentration device according to the present invention is used in purification and/or concentration of a compound such as endocrine disturbing chemicals, agricultural chemicals or pharmaceuticals contained in gas or liquid and, in any of these cases, can attain the object quickly in a short period of time.

Claims

1. A compound purification-concentration device, which has a packing material for purifying and concentrating a compound and a fluid permeating plate for holding the packing material at each end surface of the packingmaterial in a container having an inflow port and an outflowport for a fluid, being characterizedby having a space portion at an outer surface of the fluid permeating plate at each end surface.

2. The compound purification-concentration device as claimed in claim 1, comprising a projected structure for holding the fluid permeating plate on an inner side surface of the container at the outer surface side of at least one fluid permeating plate.

3. The compound purification-concentration device as claimed in claim 1, wherein an inner wall of the container at the outer surface side of at least one fluid permeating plate has a tapered structure.

4. The compound purification-concentration device as claimed in claim 1, wherein a material which does not affect the purification-concentration of the compound is packed in the space portion.

5. The compound purification-concentration device as claimed in claim 4, wherein the material which does not affect the purification-concentration of the compound comprises one or more members selected from the group consisting of a glass particle, aglass fiber, aquartzparticle, aquartz fiber, aceramicparticle, ametallicparticle, ametallic fiber, apolymerparticle, apolymer fiber, gravel and sintered articles thereof.

6. The compound purification-concentration device as claimed in claim 1, comprising a groove-like structure at the outer surface side of at least one fluid permeating plate.

7. The compound purification-concentration device as claimed in claim 6, wherein the groove-like structure is provided on an inner wall of the container.

8. The compound purification-concentration device as claimed in claim 1 or 4, wherein a volume of the space portion at one side is 0.2 to 50% of an entire volume, while a total volume of the space portions at both sides is .0.5 to 50% of an entire volume.

9. The compound purification-concentration device as claimed in claim 1, wherein the packing material is a monolith (rod-like porous continuous body) or in a fiber form.

10. The compound purification-concentration device as claimed in claim 1, wherein the packing material is in a spherical form, crushed form or amorphous grainy form having an average particle diameter of 5 μm or more.

11. The compound purification-concentration device as claimed inclaiml, 4orlO, whereinthepackingmaterialcomprisesamaterial which undergoes change in volume by coming in contact with the fluid.

12. The compound purification-concentration device as claimed in claim 11, wherein the volume change rate of the packing material is 0.5 to 50%.

13. The compound purification-concentration device as claimed in claim 1, being in a form of a cartridge or a column for solid extraction.

14. The compound purification-concentration device as claimed in claim 1, wherein one of the inflow port and the outflow port has a male structure and the other has a female structure capable of being coupled with the male structure.

15. The compound purification-concentration device as claimed in claim 1, being designed such that when the fluid is a gas and is flown at a flow rate of 6 to 12 L/min, a linear velocity of the gas which passes through a side face of an imaginary column formed by a plane which is vertically dropped from a peripheral line of the inflow port or the outflow port of the fluid to the surface of the fluid permeating plate is to be 30 m/sec or less.

16. Amethodforpurifyingandconcentratingacompoundcontained in a fluid, being characterized by using the compound purification-concentration device as described in any one of 1 to 15 above.

17. The method for purifying and concentrating a compound as claimed in claim 16, wherein the compound comprises one or more members selected from the group consisting of an environmental pollutant, dioxins, endocrine disturbing chemicals, agricultural chemicals, a surfactant, abiotoxin, a natural medicine, a natural coloring agent, a natural fragrance and a natural seasoning.

18. The method for purifying and concentrating a compound as claimed in claim 16, wherein the fluid containing the compound is in the form of liquid and/or gas.

19. The method for purifying and concentrating a compound as claimed in claim 18, wherein the liquid is selected from among an environmental water, a biological fluid, a separated liquid, an extracted liquid and an absorbed liquid.

20. The method for purifying and concentrating a compound as claimed in claim 18, wherein the gas is selected from among an atmospheric air, an indoor air, a separated gas and an extracted gas.

21. A method for purifying and concentrating a compound in a gas sample, wherein the gas sample is flown by using the compound purification-concentration device as claimed in any one of claims 1 to 15 at a flow rate of 6 to 12 L/min such that a linear velocity is to be 30 m/sec or less when the gas passes through a side face of an imaginary column formedby aplane which is verticallydropped from a peripheral line of the inflow port or the outflow port of the fluid to the surface of the fluid permeating plate.