TWI237578B - Fiber matrices dispersed with dehydrating agents, manufacturing processes thereof and columns for cleanup using the same - Google Patents

Abstract

The present invention aims to provide a device for dehydrating samples having a dehydrating function by way of a dehydrating agent, which is easy to use for a cleanup column and a cleanup column comprising said device. Fabric matrices which have been washed using organic solvents without the dissociation of components interfering assay dispersed with at least one dehydrating agent selected from sodium sulfate, sodium carbonate, sodium chloride, silica gel, alumina, magnesium sulfate, calcium sulfate, calcium chloride, copper sulfate, potassium carbonate, calcium oxide and the like, for dehydrating samples, a manufacturing process thereof and a cleanup column using said device are provided.

Description

1237578 IX. Description of the invention: [Technical field to which the invention belongs] The present invention relates to a fiber matrix for dehydration (fibre legs) containing a chemical = qualitative sample that will be the object of separation and quantitative analysis, and a method for manufacturing the fiber. And a purification column using the fiber matrix. [Previous technology] When separating and quantifying chemical substances, it is generally necessary to remove and quantify the desired chemical substance in advance to remove it from the sample in advance. · For prejudicial or disturbing compounds, a pretreatment is usually performed. This pretreatment is called a clean-up operation or purification process. In order to improve the accuracy of the separation. _ Quantitative analysis is widely used. This purification operation is especially necessary for microanalysis. For example, in the samples used for the analysis of dioxin obtained from the environment, in addition to coexisting multiple organic compounds, the amount of dioxin only exists. To a trace level of 1 (M5). Therefore, if a high-precision and quantitative separation is performed, Nichi ''s gas chromatography (Gc: ^

Chromatograph) / f if ^ (MS: Mass Spectrograph) # ^, ^ At this stage, a purification operation must be performed to remove dioxin analysis: the compound that hinders or 々 # is used to remove the compound and dehydrate the sample. Appliances, ie devices, are necessary. Fill in with carbon ##, and use active traits to absorb energy, such as dioxins, which have a flat structure (Planar) structure. This effective knife dioxins and other organic compounds can be processed before dioxin analysis. Purification operation in ”(revised version) 314038 5 1237578 Generally, in the purification operation using an activated carbon-containing filler, after loading the sample into the column, hexane or containing 25% (v / v): Hexane (the first liquid) of chloromethane flowed through the column and the inclusions were dissolved out of the column to remove, and then toluene (the second liquid) was flowed through the column and the dioxin was dissolved for classification. Known methods for passing liquid include a method in which both the hexane of the first liquid or hexane containing 25% (v / v) of digas methane and the toluene of the second liquid are passed from one direction of the column ( A liquid passing method A) and a method in which the first liquid is passed through the tube string and the second liquid is passed through the tube string in the opposite direction (reverse flow).

Commonly referred to as liquid-through method B, dioxin can be dissolved from the column with a small amount of toluene (second liquid). As a result, the advantages of shortening the time for passing through toluene and the time for concentrating the secondary process can be obtained. In addition, since the concentration ratio is reduced, contamination caused by toluene in a liquid-passing solvent is reduced, which is an advantage. Furthermore, there is an advantage that a high recovery rate can be easily obtained. The string used in the liquid-passing method A is described in the Japanese industrial standard "Measurement Method for Dioxins and Cobrana Polychorobiphenyl in Exhaust Gas", and is a glass string The bottom of the chromatograph tube (inner diameter 10mm) is filled with quartz glass wool, and on top of it is filled with sodium sulfate with a thickness of about 100 Å and activated carbon-containing filler 1 g, with a thickness of about 100 Å. Produced by. On the other hand, the column used in the liquid-passing method B is, for example, William et al. (David T. Williams et al., Chemosphere, 22, 1019 (1991)) (Davier William et al., Actinic layer, Volume 22, page 1019 (1991)), is filled with a filler containing activated carbon in a glass tube, and (revised) 314038 6 1237578 is filled with sodium sulfate at both ends, and then filled with glass wool to make . Also, as described in Smith (L.M. Smith, Anal. Chem., 53, 21 52 (1 981)) (L.M. Smith, Analytical Chemistry, Vol. 53, p. 2152 (1981)), The glass tube is filled with a filler containing activated carbon, and fiber filter paper is filled at both ends thereof to make it.功能 The function of sodium sulfate used in the production of the official column is to remove the water contained in the sample solution packed in the official column and the water contained in the organic solvent that is used to pass the liquid. Sodium sulfate will absorb water and change from anhydrous salt to working water salt. If the sample solution or organic solvent containing water is directly passed through the activated carbon filler layer of the column without dehydration treatment, it will affect the activated carbon.

Adsorption force, and there will be concerns about abnormal segmentation. Furthermore, in the liquid passing method A, the sodium sulfate layer on the activated carbon-containing filler layer has a function of preventing disturbance of the front end of the activated carbon-containing filler layer caused by the dripping of the solvent. In addition, active carbon-containing fillers are well-known as activated carbon-dispersed silicone rubbers obtained by mixing activated carbon with silicone (Wakimoto et al. (Τ · Wakimota, etal,

Chemosphere, 27, 21 1 7-2122 (1 993)) (T. Wakimoto et al., Chemosphere, Vol. 27, pages 2117 to 2122, (1 993)), Japanese Patent Application No. 2000- 121554) [Products of Kanto Chemical Co., Ltd.]. It is also known that activated carbon embedded in silicon gel produced by the action of a mixture of sodium silicate (water glass) and activated carbon with an inorganic acid (Japanese Patent Publication No. 7-50084) [Wako Pure Chemical Industries, Ltd.] Products]. For activated carbon-containing fillers, Carboxen 1 000, 1 〇16 7 (revised version) 314038 1237578 revers i bi e tube filled with carbon molecular sieve is well known [ Hikma Altoliji's products (shared daggers)] (Matsumura Chiri et al. (7th Environmental Chemistry Symposium Lecture Series, No. 154 (1998)). This is the inside of a polypropylene column Filled stone anti-molecular division, and by filling polyethylene ends with 溏 'organs at both ends, it can be used in = Method B. But' the column is not filled with sodium sulfate, so ... Removal function. Also, the filter has poor liquid permeability, especially

In the case of an organic solvent, there is a concern that a component made of polypropylene and a filter made of polyethylene may dissolve a component that prevents analysis, which is a problem. Also, the conventional filler-containing filler column has the following disadvantages. $ Only filled with activated carbon-containing fillers and not filled with sodium sulfate = Nishou 'Because the sample solution packed in the column and the organic solvent towel used as the liquid 2 can not be removed, the result will be It affects the adsorption of activated carbon, so that there is a doubt that it cannot be correctly divided. 0 Laminate sodium sulfate on the filler layer containing activated carbon, and laminate glass fiber (including glass wool and glass fiber filter paper, the same below) on the filler layer containing ^ From the time of making the tube to the time of using the string The exciting “Gu Yi” caused the filler layer containing activated carbon and the sodium sulfate layer in the official column to be mixed with each other, and the performance of the column was impaired. ③ Put glass fiber on the filler layer containing activated carbon, and when the glass fiber is laminated on the layer of sodium sulfate, if compared with ②, the filler layer containing activated carbon and sodium sulfate are less likely to occur when compared with ② Layer movement and mixing cannot be completely prevented. In addition, although it can be sold freely, although ..., the glass fiber layer is added to improve the effect of suppressing the movement and mixing of the filler, but it is not practical as the liquid permeability of the column decreases. . (Revised version) 314038 8 1237578 ④ If glass fiber is not used, A &T; T (material (such as plastic), human strength filter, device) can improve the movement of the filler. When using organic solvents, the doubts about the components that hinder the analysis from the filter (such as plastic " θ) are a matter of content. [Summary of the invention] A question. Therefore, the above-mentioned conventional techniques should be used. In terms of the problem, the present invention provides a device for dehydrating the water generated by a dehydrating agent, which is used for purifying the daggers and daggers. ; 仏 $ This equipment is used for purification. The method of the problem is ^ g_ In the repeated research, the liquid agent has been found to be used only by dispersing and decoupling. I:: The device is unexpectedly possible. -Complete the results of this research and 'eight in repeated research, and finally that is, the present invention is about dehydrating agents in organic or inorganic fibers washed with organic solvents instead of ^ = used to dehydrate the sample Fiber-based f, the aforementioned ^ 酉 夂, sodium carbonate 'sodium chloride, Μ Μ is selected from at least one of & calcium chloride, iron oxide, stone mountain, aluminum chloride, stone "magnesium, calcium sulfate, copper oxide inverse acid removal, oxidation reduction, etc." Also, the present invention is With regard to Yihuohao, +, the fiber is a glass fiber, and all fiber matrices are characterized by: F is selected from Meng fiber or mineral fiber. In particular, the present invention relates to a dehydrated sulfur. ^ 之 林基贝, It is characterized by: (Revised version) 314038 9 1237578 The present invention relates to a method for producing a fiber-based f, which contains a sodium sulfate, a sodium carbonate, a sodium carbonate, a dream gelatin, an oxide, and a sulfate Process of selecting at least one kind of dehydrating agent solution including sulfur, sulfur chloride, copper sulfate, potassium sulfate, potassium potassium, oxygen osmium, etc., washing with an organic solvent without dissolving out the organic fiber-based f or inorganic fiber matrix of the obstructing component (2) The above-mentioned fiber matrix impregnated with the dehydrating agent solution is dried, and the present invention relates to a tubular column for hydration ^ Dan Xingzhengma........ Furthermore, the present invention relates to one of the aforementioned purifications: The column packing agent is a silicone gel containing activated carbon. ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, The purification column of the aforementioned, which: The sample contains dioxin. The fibrous matrix is novel and can be used as a net. 'It can be used for liquid and gas drying. If its purpose is to be used for liquid or gas drying, then 1 should be planted on the right / its 4+ Α — it does not matter. It can be applied, for example, Filled in the "lower part of the main color tube to remove the moisture of the sample's shape" or the liquid for organic solvents, etc. Μ: This temple can be easily removed by passing it through the aforementioned fiber matrix: And 'Because the fibrous matrix-based dehydrating agent is made of hibiscus in the matrix: Therefore, the surface area of the dehydrating agent is large, which is more than that of conventional methods. Its dehydrating effect is more excellent. Wanqian Tongli [Embodiment] The fiber material used in the fiber substrate of the present invention is not particularly limited as long as it can disperse and maintain the dehydrating agent without affecting the analysis (modified version) 314038 1237578. Broken glass fiber, ς = micro-inorganic fiber of substance is very suitable, but such as = ancient: physical fiber and so on, that is, does not cause dissolution analysis hindering components, it can also be used by the = = = media washing the fiber can be used alone, t know Mian wait. In addition, _ can be used in combination of two or more. ㈣ 其 # Lu, from the point of view of usability, especially f 义 、. 隹 基贝 和. Glass fiber, fiber, and fiber are very suitable

When using glass wool and / or breaking as a fibrous substrate, from the point of view of the fixation force on the dehydrated south j, ^^ m " ^ The diameter of the inner diameter of the broken glass domain is 20 / ^ Guangliang 1 soil 'annual inch is preferably 1 〇 # m or less. The dehydrating agent used in the present invention is not particularly limited as long as it is water-absorptive and insoluble in the organic solvent used, but it can be used: sodium sulfate, sodium enoate, sodium chloride, or silicone, alumina, Magnesium sulfate, calcium sulfate, calcium gasification, copper sulfate, potassium carbonate, calcium oxide, etc. In particular, sodium sulfate is more used. In the present invention, the chemical substance that is the object of separation and quantitative analysis is not particularly limited. Generally speaking, it can be exemplified by polychlorinated dibenzo-p-dioxadiene, Dioxins of gaseous dibenzofuran and PCB · Polychorobiphenyl. Others can also be applied to organophosphorus compounds such as polychlorinated biphenyls (PCB), Acephate, Diazinon, Dichlorvos, Malathion, Trichlorfon, etc. Carbary 1, ISOprocar 3), Dianweiwei (revised version) 314038 11 1237578 (Thiobencarb), Aldicarb, and other amino esters, Propanil Etamines, ureas such as Dimecrón, α-, / 3-, 7-, hexachlorobenzene (Bhc: benzene Hexachloride), digas diphenyl-dichloroethylene ( p, p '—DDE) and other organic gases, pyrethrins such as Cyf iutrin, Cypelmetrin, Cyhaltrin, and triacetazole ( Tricyclasol), Propicones (Própiconasi) and other agricultural compounds such as nitrogen, polycyclic aromatic compounds such as anthracene, benzopyrene, pyrene and naphthalene, polychlorinated biphenyls (PCB) ), Polybrominated biphenyls, pesticides, alkylphenols, bisphenol A,% chlorophenols, phthalates, di-2-ethylhexyl adipate, benzo [a] pyrene, two Methanone, 4-nitrotoluene dimer, styrene trimer, outside the group tributyl tin compounds, triphenyl tin compounds and other sexual endocrine disturbing chemicals (i.e. environmental hormones) or the like of chemical substances. For example, when purifying chen medicines, as described in "Tap Water Test Method 1 993 Edition (Japan Water Association)", in order to remove inclusions from the measurement sample in the first stage of gas chromatography measurement, use Red block g South Territory or Silicone for purification operation. The red block kaolin column chromatography tube used for the purification operation was prepared by filling 8 g or 20 g of red block kaolin in a glass column chromatography tube and depositing 4 g of sodium sulfate thereon. In the same manner, a silica gel column chromatography tube was filled with 8 g of silica gel in a glass column chromatography tube, and 4 g of sodium citrulline was deposited on the glass column chromatography tube to make ′. For example, in Chiosrpyri (〇s), ebion (EPN), Isopröthlslam, Captan, τρΝ, TοluchlOPh〇smethy (Etridlazole), Chloranil, prOpyzamide, (revised) 314038 12 1237578-ethalln, Benfluralin, Demeton, and total pesticides (CNP) In a similar purification operation, the column chromatography tube containing 8 g of red block Nanling clay was filled with the sample solution, and 20 ml of burned solution was passed through and the effluent was discarded. 50 ml of hexane was passed through and the effluent was discarded. Finally, 15% (V / V) propane and hexane 1_1 were passed through, and the effluent was concentrated for gas chromatography.

The method for manufacturing the fiber matrix for dispersing the dehydrating agent according to the present invention includes a method of dispersing the solid, dehydrating agent directly in the fiber matrix, or the process of ⑴ = breaking the fiber matrix, and The method of drying the fibrous substrate, as long as it can be = water material ㈣ dispersed surface wiki # towel, there is no specific limit ▲ For the solvent of the dehydrating agent solution, for example: water, methanol, ethanol And acetone, etc., but there is no special limitation. However, from the viewpoint of solubility, cost, and safety (ignition, explosion, etc. are better for the human body and the king. Brother's shirt ring), water makes the immersion in the dehydration. The fibrous matrix of the agent solution is heated • dehydrated, air-dried, and reduced-house-dried = dissolved in glass fiber, and then kept in glass fiber ^ two will be stabilized at a temperature above 10 For the sake of drying ^, it is more ideal. Change to anhydrous salt. ^ When the dehydrating agent solution is used to disperse the sodium sulfate of 10 water salt, the amount of dehydrating agent solution of the opposite fiber (including glass (revised version) 3] 4038 13 1237578 cotton and glass fiber filter paper, the same below), It is preferable that the dehydrating agent Luoye can dye the whole glass fiber. For example, using glass fiber filter paper GA200 (manufactured by Adu-Fandic Toyo Co., Ltd.) and sodium sulfate Nissho, a glass fiber filter paper of 900 cm2 in sodium sulfate aqueous solution (maximum concentration: 21.9% (25.0%). The appropriate amount of) is about. At this time, the adjustment of the amount of sodium sulfate dispersed and adhered in the glass fiber can control the change in the concentration of the sodium sulfate aqueous solution. The amount of the sodium sulfate aqueous solution can disperse the sodium sulfate into the glass. The fiber full penetration P can not only lose sodium sulphate if it is added too much. When the glass is dried or cut, Gu easily segregates in sodium sulfate in the glass fiber. That is, more sulfur is precipitated in the lower part of the glass fiber. On the other hand, if the aqueous solution of different sodium sulfate is directly mixed with the solid sodium sulfate and the fibroin domain to disperse it, from the degree of dispersion, the glass = two of: From the point of view of power and dehydration ability, it is preferable to use sodium sulfate as the most reasonable. It is called w. 3. The particle diameter is made into the fiber matrix of the following dispersing dehydrating agent (dehydrating agent-dispersed fiber-based shell): it is filled before F on processing column At least one end of the filler is in contact with the dehydrating agent to disperse the fiber matrix and the column filler. The two columns of the dehumidifying solution or the solvent are used to dissolve the fiber matrix by injecting the sample into the g column. (Revised version) 314038 14! 237578 The column / packing agent for separation and quantitative analysis is not particularly limited, but it can be appropriately selected according to the fact that active substances containing active stone mountains can be used. Specifically, ", Activated carbon filler, driving and oxidation filler. Shuotu Temple is well-known—filling a column with chemical substances as the object of analysis is the point of view. From the viewpoint of inhalation, activated carbon-containing fillers such as II㈣ are preferred.

From the point of view, it is better to use the shell as a beam, from the absorption property, the work piece back to the territory, silicon rubber, graphite carbon, etc. If the chemical substance to be analyzed is an exogenous endocrine disruptor: (also% hormonal), from the standpoint of adsorption, red-tailed territories, silicone, and graphitic carbon are preferred. The shape of the official column used in this month is not particularly limited, as long as the fiber soil shell can be fixed in the glass tube, it can be used whether it is linear or gourd-shaped. ^ The material of the column used in the present invention is not particularly limited as long as the organic solvent does not reveal the components that hinder the analysis during liquid passing, and glass, stainless steel, Teflon, etc. can be used. [Examples] Examples of the present invention will be described below to specifically explain the present invention. However, the present invention is not limited to the following examples. iMJH 1 (1) Preparation of Silicone Filler with Activated Carbon in Silicone 60 (Spherical, 100 to 210 // m) (Kanto Chemical Co., Ltd.) 15 (Revised) 314038 1237578 $ 中 = 、 加 经The whole granule is activated carbon below 38 m (Kanto Chemical Co., Ltd.) and uniformly mixed. Then, it is heat-treated under a nitrogen flow (500ml /) at 400 ° C for 1 hour to prepare activated carbon-containing silicone. Filler. (2) Preparation of glass fiber filter paper dispersed with sodium sulfate After washing the glass fiber filter paper with acetone at 2000 (Toyo Ado-Fantic (also) clothing), dry the mixture. Adjust the concentration 丨 · 6.8 mol / liter of sodium sulfate aqueous solution, add 2% of each glass fiber filter paper of 900 cm2, add [...] sodium sulfate aqueous solution described above, and wet the glass fiber filter paper GA2OO as a whole. Inside the machine, it is dried for 6 hours at 130 ° C to produce glass fiber filter paper with dispersed sodium sulfate. (3) Activated carbon glass column is made in the center of a glass tube with an inner diameter of 8mm and a length of 140mm, in order from below Rolled through glass fiber filter paper GA2⑽ (9_χ 5⑽m) dispersed with sodium sulfate ( The width of the glass fiber filter paper layer: 9mm), then, filled with silicone gel containing activated carbon, and finally plug the glass fiber filter paper GA2OO (9mm x 50mm) dispersed with sodium sulfate (the width of the glass fiber filter paper layer ... 9_) to make a column. Here, a glass fiber filter paper GA 2 0 (9mm x 50mm) contains about 0.12g of sodium sulfate in a dispersed state, and absorbs up to about 0.15g of water. As an endurance test on the amplitude of a string, a handy type vibrator (for glass columns) (gier science) is used on the string prepared by the method described above. Shake for 10 minutes, then use the shaker-SA_31 (made by Yamato Scientific Co., Ltd.) to give the pipe a vertical direction (revised version) 3M038 16 1237578 ::: ...! Minutes (intensity scale: 5), As a result, the silica containing activated carbon in the column did not leak to the outside of the glass fiber filter paper at both ends. Of course, the "containing live rabbit" and sodium sulfate have not been mixed. The durability of activated carbon frit is quite high. X (4) Partition test for activated carbon glass column packing containing ^ 5ml of a sample solution (solution: hexane) of tetrachlorobiphenyl terephthalate (IPPm) and OCDD (octabibiphenylene dicarbadiene) (10PPm), and then using hexane 0.5ml rinse the inner wall of the column. Here, among the dioxins, polychlorinated biphenyls (PCDD) (4 to 8 chlorides) and polychlorinated biphenyl sulfonium (F) to 8 chlorides, 136 8_TCDD belongs to the earliest dissolution type, and the other 0CDD belongs to the latest dissolution type. Secondly, on the activated carbon glass column, a linear reservoir made of Teflon was used to connect a glass reservoir, and a 200 ml separatory funnel was connected thereto. Next, a separation funnel was charged with 150 ml of hexane containing 25% (v / v) dichloromethane, and the liquid was passed through the column. Then, the activated carbon glass column was turned and reconnected, and toluene was placed in a separating funnel, and toluene was added to 300 ml ′ to allow liquid to flow through the official column (50 ml x 6). The flow rate is the same as 2.5 ml / min. 2.5 to 2.5 ml / min., Which is the same as the method for measuring dioxin and cobrana pa in the exhaust gas of the industry standard L. Each fraction was concentrated to 100 # 1, and then analyzed by HRGC (PackaiOMQOID-MS (Modlebka 5971)) sequential ion mass spectrometry (SIM Secondary ion mass spec 1: roscopy) analysis, To check the dissolution pattern of dioxin. (Revised version) 3M038 17 1237578 Figure 1 shows the results of the division test. From Figure 1, it can be seen that the dioxin and dioxin did not dissolve in the gas containing 25% (v / v). In the hexane separation, it is only eluted in the second benzene separation, and has excellent separation function. In order to dissolve 〇CDD with high affinity to activated carbon from the column, the solution is passed through from one side. In the method, 200 to 300 ml of toluene is usually required. In contrast, if the column is inverted and the liquid is passed through, OCDD can be dissolved out with only a small amount of toluene below 50 ml. Example 2 (1) Containing Preparation of activated carbon silicone filler was prepared in the same manner as in Example 1. (2) Preparation of sodium sulphate-dispersed glass wool The glass wool (glass fiber diameter 1 to 6 / zm) was washed with acetone and dried. A mortar was used. Pulverize sodium sulfate (anhydrous) (made by Kanto Chemical Co., Ltd.) 2. The above 5.0m of glass wool was fully mixed to disperse the sodium sulfate powder in the glass wool. (3) Preparation of activated carbon glass pipe column with an inner diameter of 8mm and a length of 140mm, at a distance of 34 mm from both ends (2 Where) there is a gourd-shaped glass tube, between its narrowness and narrowness, from the bottom is filled with 0.14g of glass wool with sodium sulfate loose (the width of the glass wool layer: about 15 bands), and then, filling Silica gel containing activated carbon lg. Finally, 0.14 g of glass wool dispersed with sodium sulfate (the width of the glass wool layer: about 15 mm) was filled to make the official column. Here, one glass wool was dispersed. Contains about 0.04g of sodium sulfate, and has the ability to absorb up to about 0.05g of water. As a long-term test on a vibrating string, it was prepared (revised) 314038 18! 237578 by the above method. On the pipe string, use a convenient vibrator (for glass pipe string) (made by Gier Scientific Co., Ltd.) to give vibration for 10 minutes, and then use an oscillator (Shaker_sA_3i) (manufactured by Yamato Scientific Co., Ltd.) to give the pipe column a vertical direction. Vibration was 30㈣ (intensity scale: 5). As a result, the column contained activated carbon. Never leaked to the outside of the glass wool at the ^ end. Of course, activated carbon cutting glue and sodium sulfate have not been mixed. The durability of activated carbon glass tubing to vibration is quite high. (Scribing test) m to activated carbon glass tubing Fill with a simple material containing ^ ㈣ 闻 ㈣ and OCDD (H) 卿 (solving hexahedron), and then rinse the inner wall of the column with 0.5ml of hexane. 2. Next, on an active glass column, Made of Teflon linear coupling to connect glass M, and a fine MI separatory funnel. ㈣Second ', a separatory funnel was charged with 25% (v / v) dichloromethane in a m mf 对 f * column. Next, turn the activated carbon glass column and sell a new connection. Place toluene in the separatory funnel, add toluene to it, and make it 30- to make the column flow through (mlx 6). The flow rate and the measurement method of dioxin and coplanarium in industrial-specific exhaust gas are two pounds: 2.5inl / min. Of the same degree of 20 to 2.5mi / min. Each of the 4 waves was reduced to IGGml, and then analyzed by the method of hearing (Supleka 5_ = white card 59 (sequential ion mass spectrometry)) to detect the dissolution pattern of ausin. ’From the results of the reticle test (Figure 2), it can be seen from the examples! Feelings open =, dioxins are not dissolved in 25% (v / v) m ^ knife, but only in fx, ^ 7 in this area, with excellent separation 具有 (revised version) 314038 19 I237578 / 4 〇V7 sr The OCDD with high affinity to activated carbon is dissolved from the column ^ In the method of permeating liquid in one party, usually 200 to 300mi of the former is required. When the liquid is reversed and passed through, OCDD can be dissolved out with only a small amount of toluene less than 50 ml. [Effects of the invention] According to the present invention, it is possible to realize that the packing material in the column does not move or mix due to vibration, etc., has the function of removing moisture, has good liquid permeability, and performs chemical substances with excellent separation performance. Especially the analysis of dioxin. [Brief Description of the Drawings] FIG. 1 is a diagram showing the dissolution behavior of dioxin in Example 1. FIG. FIG. 2 is a diagram showing the dissolution behavior of dioxins in Example 2. Table 0 (revised version) 314038 20

Claims (1)

1232 (578 ^^! L :; ..... 10. Patent application scope ... The seed fiber matrix is washed with an organic solvent without elution analysis. The dehydrating agent is slightly omitted in the organic or inorganic fibers that prevent the formation of ^ 7 are uniformly dispersed to dehydrate the sample. The aforementioned dehydrating agent is composed of sodium sulfate, carbon 'sodium chloride, silicone, alumina, magnesium sulfate, calcium sulfate, 2 calcium chloride, copper sulfate, and potassium carbonate. At least one is selected from the group consisting of calcium oxide, calcium oxide, and the like. Σ T The fiber matrix of the first patent scope, wherein the fiber is a glass fiber, a metal fiber, or a mineral fiber. I ★ The first or second patent scope of Shenqiao The fibrous substrate, wherein the dehydrating agent is sodium sulfate. A method for producing a vitamin substrate comprises the following steps: sodium sulfate, sodium chloride, silicone, alumina, magnesium sulfate, calcium sulfate, At least one selected from calcified calcium sulfate, steel sulfate, potassium carbonate, calcium oxide, etc. "= aqueous solution immersed and washed with organic solvent without dissolution analysis hinders the process of organic fiber matrix or inorganic fiber matrix, and ( 2) Before the impregnation with 2 dehydration solution The fibrous matrix carries money ㈣ On one end side, a fiber-based medium with “string filling” sample is a kind of purification string containing at least one of the string fillers as in any of the items 1 to 3 of the scope of patent application. For example, the purifying column for item 5 in the scope of patent application, its M is a second gel containing activated carbon. For example, the purifying tubing string under the scope of application for patent β includes dioxin. 〃 (Revised) 3M038 21