KR101507042B1 - Extraction kit using setting device of a sample for accelerated solvent extraction - Google Patents

Extraction kit using setting device of a sample for accelerated solvent extraction Download PDF

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KR101507042B1
KR101507042B1 KR20140152571A KR20140152571A KR101507042B1 KR 101507042 B1 KR101507042 B1 KR 101507042B1 KR 20140152571 A KR20140152571 A KR 20140152571A KR 20140152571 A KR20140152571 A KR 20140152571A KR 101507042 B1 KR101507042 B1 KR 101507042B1
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sample
extraction
extraction kit
cap
ring
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KR20140152571A
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Korean (ko)
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최민규
이인석
황동운
백승홍
윤세라
정래홍
김상수
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대한민국
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction

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  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample setting means used for extracting a sample liquid required for analyzing a specific component from a sample by using an accelerated solvent extractor (ASE), and more particularly, A sample inlet pipe of a transparent material inserted into the extractor body of the extraction kit, a buffer sealing ring arranged at the upper and lower ends of the sample inlet pipe, and a sealing ring inserted into the inner periphery of the lower end of the sample inlet pipe, By providing the sample setting device including the filter support ring, it is possible to visually confirm the operation of putting the adsorbent of the interference material and the sample sample in a laminated manner to the upper side of the fiber filter, so that the injection and setting operation of the sample can be performed more accurately , Which makes it possible to optimize the composition of the sample liquid extracted from the accelerated solvent extraction apparatus, In addition, since only a low-cost sample setting device can be used as needed in a state in which contamination occurring in the expensive extraction kit is minimized, the service life of the extraction kit can be maximized and strong acidity or strong basicity It is also possible to use economical and reasonable extraction method which can use up to adsorbent treated with 34mL. Also, it is possible to use 22mL of inner volume extraction kit and to improve the compatibility of extraction kit. To a solvent extraction kit.

Description

[0001] The present invention relates to an accelerated solvent extraction kit equipped with a sample setting device,

The present invention relates to a sample setting means used for extracting a sample liquid required for analysis of a specific component from a sample by using an accelerated solvent extractor (ASE) And a filter support ring inserted into the inner periphery of the lower end of the sample inlet tube to support the fiber filter. The filter injection device according to claim 1, By providing the sample setting device, it is possible to visually check the operation of putting the adsorbent of the interfering substance and the sample sample in a laminated manner on the upper side of the fiber filter, so that more accurate sample input and setting operation can be performed, The present invention relates to an accelerated solvent extraction kit equipped with a sample setting device for preventing corrosion of an extraction kit even if a treated adsorbent is used All.

As a part of analyzing the marine environment by monitoring various oil pollutants including polycyclic aromatic hydrocarbons (PAHs), the process of preparing the sample liquid for analysis of oil pollutants from the marine sediment is usually performed in several steps due to the complexity of the matrix However, in order to obtain a reliable analysis result of oil pollutants, it is most important to extract the sample liquid from the marine sediment and to purify and concentrate the extracted sample liquid.

As a method of extracting the sample solution for analysis of oil pollutants from the marine sedimentation soil as described above, a typical extraction method using an accelerated solvent extraction apparatus (ASE) A method of extracting a sample by using an organic solvent to enhance permeability and material transporting ability of a sample and to maintain an organic solvent having a boiling point or higher in a liquid state at a high density using a high pressure (1500 psi or more) US Environment protection agency for the analysis of organic pollutants present in various solid samples.

FIG. 1 schematically shows the structure of an accelerated solvent extraction apparatus. As shown in FIG. 1, there are shown a plurality of (generally two or three) solvent storage vessels 1 in which a solvent is stored, A mixing valve 2 for mixing the solvent discharged along the supply line 1a at a specific ratio and a solvent supplied through the mixing valve 2 through an extraction kit A heating oven 4 for heating the extraction kit 10 and a heating unit 5 for heating the sample discharged from the extraction kit 10 along the sample extraction line 5a, And a sample storage container 5 for storing the sample.

The extract kit (10) is 22mL, 34mL, or the information three types that has the product of 66mL mainly used, and using the stainless steel material is made of the extractor body and the same material is made of a cylindrical form onto the extractor body, the lower end The upper and lower caps are respectively provided with an upper cap and a lower cap which are assembled and installed on the upper and lower caps, respectively. The inner bottom of the extractor body is provided with a fiber filter for supporting a sample sample and filtering impurities when extracting the sample liquid. A solvent injection port and a sample liquid extraction port are respectively formed.

Therefore, a sample sample of the lyophilized marine sediment is introduced into the extraction kit 10, and then the extraction kit 10 is discharged from the solvent storage container 1 in a state in which the extraction kit 10 is installed in the accelerated solvent extraction device The solvent is mixed at a certain ratio using the mixing valve 2 and then the solvent is pressurized and injected into the interior of the extraction kit 10 using the injection pump 3 and the extraction kit (10) is heated to a predetermined temperature, the solvent injected into the extraction kit (10) is passed through the bottom side fiber filter together with the oil contaminant component contained in the sample sample under the condition of high temperature and high pressure, Is extracted.

The accelerated-solvent extracting apparatus shown in FIG. 1 and the extraction kit 10 used therein are used not only for extracting a sample liquid for analysis of oil pollutants from various soil samples including marine sediment, A well-known apparatus widely used for extracting analytical components contained in a sample is a product manufactured and sold under the model name ASE 350 by Dionex Corporation of USA.

However, in the conventional extraction method using the accelerated solvent extraction apparatus, after the sample liquid is firstly injected into the extraction kit 10 to extract the sample liquid, the lipid component, the sulfur component and / or the pigment component and the cholesterol component A sample refining process that removes various interfering substances contained in the sample sample that cause difficulties in analyzing the oil pollutants with several adsorbents, and a problem in which a concentration process of filtering out the adsorbent from the purified sample liquid and concentrating the same .

In other words, several additional steps of extraction, purification and concentration of the sample liquid are performed separately before the actual sample analysis step by gas chromatography-mass spectrometry determination, There is a problem that the reliability of the analysis result is lowered due to the volatilization or loss of the pollutant component and the time required for securing the sample liquid is unnecessarily delayed, There is a problem that it takes a long time.

In order to solve the above-described problems, it is an object of the present invention to provide a method and apparatus for extracting a sample liquid for analyzing contaminants from a sample using an accelerated solvent extraction apparatus, (1-step) extraction and purification method is proposed by the present applicant as a patent application No. 153759 filed by the applicant in 2013 (No. 10-1421077).

According to the above-described prior art, before the sample is introduced into the extractor body of the extraction kit for accelerated-solvent extraction apparatus 10, the adsorbent of the interference substance, which has been applied to the existing purification step, And then a sample setting method of injecting a sample sample into the upper part of the adsorbent layer enables one-step extraction and purification of the sample liquid.

However, since the extraction kit itself is made of a stainless steel material in the prior art, it is necessary to insert several kinds of adsorbents into the extractor body of the extraction kit in a laminar manner, and to put a sample in the upper part of the adsorbent layer There is a problem that it is difficult to set the adsorbent layer and the sample sample layer to a precise layered structure in accordance with a required position.

When the adsorbent components are mixed with each other or the adsorbent component and the sample sample components are mixed with each other without being precisely set in a layered structure in accordance with the positions required by the adsorbent and the sample to be injected into the extraction kit as described above, It is difficult to smoothly remove and concentrate the interference substances in the extraction process of the sample solution using the extraction device. Accordingly, there is a problem that the composition of the extracted sample solution becomes rather uneven and the reliability of the analysis result is lowered there was.

In addition, since the sample containing the organic solvent component and the adsorbent remain in the extraction kit for extracting the sample liquid, the following extraction operation must be performed after removing the sample and the application of the high temperature and high pressure Accordingly, the sample surface and the adsorbent component are strongly adhered to the inner surface of the body of the extractor together with the organic solvent component in the form of a coating layer, thus requiring a complicated cleaning operation for the extraction kit. Thus, the extraction kit, which is relatively expensive, There is a problem that the service life is shortened.

In order to increase the removal efficiency of various interference substances present in the sample, it is necessary to use an adsorbent treated with strong acidity or strong basicity. However, when an adsorbent of such a component is used, the stainless steel- And the use of strong acidic or strongly basic adsorbent would increase the economical burden of purchasing and using expensive expensive acidic and strong basic extraction kits separately.

On the other hand, observing the color and the extraction path of the sample liquid in the fiber filter in the extraction process of the sample liquid, it is relatively easy to judge whether or not the extraction operation of the sample solution is performed correctly. However, It is difficult to observe or judge the extraction state of the sample liquid. In addition, all three types of extraction kits having a volume of 22 mL, 34 mL, or 66 mL are purchased separately and used separately The economic burden and crosstalk in use are also becoming another problem.

Korea Patent No. 10-1421077

The present invention has been devised to supplement the problems of the prior art as well as contribute to the extraction and analysis of various sample solutions using the accelerated solvent extraction apparatus. It is possible to visually check the work of putting the sample sample in a laminating manner so that the injection and setting operation of the sample can be performed more accurately and the sample input and setting operation is performed in such a manner that the adsorbent does not come into direct contact with the extraction kit A buffer seal ring disposed at the upper and lower ends of the sample inlet tube; a sample inlet pipe inserted into the inner periphery of the lower end of the sample inlet tube to be inserted into the extractor body of the extraction kit, And an object of the present invention is to provide an accelerated solvent extraction kit equipped with a sample setting device including a filter support ring for supporting a sample.

According to an aspect of the present invention, there is provided a sample setting device for extracting accelerated solvent according to an embodiment of the present invention, which can visually confirm a state of a sample containing a sample and an adsorbent, A cylindrical sample inlet tube made of a transparent material so as to block the contact of the kit, and a buffer which is disposed at the upper and lower ends of the sample inlet tube to protect the sample inlet tube and prevent leakage of the solvent and the sample solution. And a filter support ring attached to the inner periphery of the lower end of the sample inlet tube to support the fiber filter.

The sample setter for extracting accelerated solvent according to another embodiment of the present invention is characterized in that the buffering seal ring used in the above embodiment is provided with a covering covering the upper end surface or the lower end surface portion of the sample injection tube, And a mounting ring which is inserted into the upper end of the sample inlet tube so as to be fitted on the inner peripheral edge or the lower inner peripheral edge of the sample inlet tube so that the mounting ring portion of the buffer sealing ring mounted on the lower end of the sample inlet tube functions as the filter support ring .

The sample setter for extracting accelerated solvent according to another embodiment of the present invention is characterized in that the upper outer circumferential edge of the sample inlet tube is formed as an inclined assembling surface that is inclined outwardly downward, A cover portion for covering an assembling slope of the sample inlet tube is additionally formed in the lower periphery of the cover, and an inner circumferential portion of the buffer seal ring attached to the lower end portion of the sample inlet tube is formed as a tapered portion having a funnel shape.

In addition, the accelerated solvent extraction kit of the present invention, to which the sample setting device is attached, includes a cylinder-shaped extractor body for injecting a sample, an upper cap assembled to an upper end of the extractor body, Wherein a solvent injection port is vertically formed in a central portion of the upper cap and an extraction kit is formed in the center of the lower cap such that a sample liquid extraction port is vertically penetrated through the extraction cap, The sample setter according to each of the illustrated embodiments is inserted into the body of the extractor so as to be detachable from the body of the extractor and firmly mounted inside the body of the extractor by fastening the upper and lower caps.

More preferably, a mounting nut for fastening assembly of the extractor body is inserted into the upper cap and the lower cap, and a fastening member for fastening the mounting nut to the upper end side and the lower end side outer peripheral edge of the extractor body, And a stopper mounting groove is formed in the upper inner circumferential portion of the lower inner peripheral portion of the upper end cap and the upper end cap of the upper end cap, and a nut stopper as a "C " Wherein a filter plate is disposed on an inner surface of an upper cap corresponding to an outlet of the solvent injection port and an inner surface of a lower cap corresponding to an inlet of the sample liquid extraction port, And a ring-shaped sealing pad for closely contacting the filter plate to the inner side surface.

According to the present invention as described above, several kinds of adsorbents are put into the upper part of the fiber filter in a laminated manner using a transparent sample inlet tube, and a work of injecting a sample sample into the upper part of the adsorbent layer is carried out visually In this way, the sample inlet tube with the sample accurately set in this way is connected to the inside of the extractor body of the extraction kit together with the buffer seal ring, It is possible to perform the extraction operation of the sample solution using the accelerated solvent extraction apparatus more quickly and accurately and to improve the reliability of the analysis result by optimizing the composition of the extracted sample solution There is an effect to contribute.

The sample inlet pipe separates the adsorbent treated with strong acidity or strong basicity from the extractor body portion of the extraction kit so that the adsorbent treated with strong acidity or strong basicity is added to improve the removal efficiency of the interference substance It is effective to prevent the adsorbent component from contacting directly with the extractor body, thereby preventing the extraction kit from being corroded by the strong acid or strong base adsorbent component and requiring an extraction kit dedicated to strongly acidic or strong basicity Provides a possible effect of extraction.

In addition, since the extraction operation of the sample liquid by the organic solvent is performed inside the sample setting unit, it is possible to minimize the contamination occurring in the expensive extraction kit when extracting the sample liquid, and if necessary, It is possible to provide an economical and reasonable extraction method that can eliminate the difficult cleaning operation of the extraction kit itself and extend the service life of the extraction kit as much as possible. It is possible to relatively easily determine whether the extraction operation is accurate by observing the color of the fiber filter and the extraction path of the sample solution.

Particularly, in a state in which a sample required for the extraction operation is set in advance in a plurality of sample setting devices, a sample setting device having been completely extracted is taken out of the extraction kit, and another sample setting device with a sample set is immediately mounted on the extraction kit, It is possible to continuously perform the extraction operation several times to several tens of times by using only one extraction kit. In addition, the sample setting device is inserted into the 34 mL volume extraction kit, It is possible to prevent an economic burden due to the purchase of a plurality of extraction kits for each kind and use of the extraction kits.

In addition, according to the sample setting device according to another embodiment of the present invention, since the buffer seal ring is directly mounted on the upper and lower ends of the sample introduction tube, the sample setting device is constituted by one assembly, According to another aspect of the present invention, there is provided a sample setting device for a simple and practical structure in which a filter support ring is not required to be additionally applied. According to a sample setting device according to another embodiment of the present invention, The upper side cushion seal ring can be maintained in a tightly closed state by the injection pressure of the sample liquid and the effect of smoothly extracting the sample solution and sufficient extraction amount of the sample solution It is possible to provide a very useful effect, such as to be able to guarantee.

1 is a schematic diagram showing a schematic configuration of an accelerated-solvent extraction apparatus (ASE).
2 is an exploded perspective view of an accelerated solvent extraction kit equipped with a sample setting device according to the present invention.
3 is a front sectional view of the assembled state of FIG. 2;
4 is a partial enlarged sectional view showing another embodiment of the sample setting device.
5 is a partial enlarged sectional view showing still another embodiment of the sample setting device.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

As shown in FIGS. 2 and 3, the sample setter 20 for extracting accelerated solvent according to an embodiment of the present invention can visually confirm the sample state of the sample 19 and the state of the adsorbent 18 A cylindrical sample inlet tube 21 made of a transparent material so as to block the contact between the adsorbent 18 and the extraction kit 10 and a cylindrical sample inlet tube 21 connected to the upper and lower ends of the sample inlet tube 21, A buffer sealing ring 22 arranged to protect the sample inlet tube 21 and to prevent leakage of the solvent and the sample solution and a filter ring 24 mounted on the inner periphery of the lower end of the sample inlet tube 21, And a filter support ring (23).

Most preferably, the sample inlet tube 21 is made of transparent glass or transparent tempered glass, and may be made of a transparent plastic material such as polycarbonate having excellent heat resistance, chemical resistance and strength, It is preferable that the thickness of the sample injection tube 21 is within the range of 0.5 to 1.5 mm so as to minimize the reduction in the volume of the sample required for sample injection while having a sufficient strength to firmly mount the sample injection tube 21 inside.

The outer diameter of the sample inlet tube 21 is substantially the same as the inner diameter of the extractor body 11 of the extraction kit 10 so that when the sample inlet tube 21 is inserted into the extractor body 11 The length of the sample inlet tube 21 is set to be in a state in which the inner surface of the extractor body 11 and the outer surface of the sample inlet tube 21 are in close contact with each other, The thickness of the cushioning seal ring 22 provided at two places is the dimension excluding the thickness.

The buffer sealing ring 22 and the filter supporting ring 23 are preferably made of a synthetic resin material having a predetermined strength and elasticity and sealing property such as Teflon resin or silicone resin, 22 and the filter support ring 23 have dimensions corresponding to the inner diameters of the extractor body 11 and the sample inlet pipe 21 and the width and thickness of the buffer seal ring 22 are set to be the same as the sample inlet pipe 21 It is preferable that the width and the thickness of the filter support ring 23 are set to a level similar to that of the buffer seal ring 22.

The fiber filter 24 can be variously applied according to the conditions of the sample liquid to be extracted and the components to be analyzed by using the accelerated solvent extraction device, and the cellulose filter or the glass fiber fiber filter is inserted into the sample inlet tube 21 by a predetermined amount to form a fiber filter layer on the basis of the filter support ring 23, (24) is also put between the sample (19) and the adsorbent (18).

The adsorbent 18 may also be applied to various kinds of impurities contained in the sample 19. For example, the adsorbent 18 may be removed from the sample 19 of the lyophilized marine sediment as described in the above- Activated carbon or the like is used as the adsorbent 18 of the sulfur compound and alumina or Florisil or silica gel is used as the adsorbent 18 of solid content including the pigment, Etc. are used.

The accelerated solvent extraction kit 10 on which the sample setter 20 is mounted includes a cylindrical extractor body 11, an upper cap 12 assembled on the upper end of the extractor body 11, And a lower end cap 13 assembled at a lower end of the extractor body 11. A solvent injection port 12a is vertically formed at a center of the upper end cap 12, The sample setter 20 of the present invention is provided with a sample liquid extracting opening 13a at the center of the extractor body 11 so as to be removable from the extractor body 11 of the extraction kit 10, As shown in FIG.

A mounting nut 15 for fastening assembly of the extractor body 11 is inserted into the upper cap 12 and the lower cap 13 and the upper end of the extractor body 11 and the lower end of the lower end A pair of rotation restricting protrusions 15b protrude from the outer circumferential edge of the mounting nut 15 and protrude from the outer circumferential edge of the upper cap 12 and the mounting nut 15, An inner circumferential portion of the lower end cap 13 is formed with a rotation preventing groove 15c into which the rotation stopping jaw 15b of the mounting nut 15 is inserted.

When the upper cap 12 and the lower end cap 13 are fastened together along the fastening portion 11a of the extractor body 11, the respective mounting nuts 15 are fastened to the upper end cap 12 or the lower end end cap 13, The injection of the organic solvent through the solvent inlet 12a is induced in the center of the upper surface of the upper cap 12 and the lower surface of the lower cap 13 in the drawing, Shaped recessed grooves 12b and 13b are formed so as to assist in extracting the sample solution through the solvent extraction line 13a and the solvent extraction line 3a and the sample extraction line 5a, Cushioning pads 12c and 13c are provided at the inner center of the recessed portions 12b and 13b.

In addition, a stopper mounting groove 16b is formed in an inner peripheral portion on the lower side of the upper cap 12 and on an upper peripheral side of the upper end of the lower end cap 13, and a release of the mounting nut 15 is formed in the stopper mounting groove 16b. And a nut stopper 16 as a C-shaped resilient frame for preventing the solvent from being injected into the inner space of the upper cap 12 corresponding to the outlet of the solvent inlet 12a and the inlet of the sample liquid extracting opening 13a A filter plate 14 is disposed on the inner surface of the lower cap 13 and a filtering plate 14 is closely attached to one side surface of the mounting nut 15 with an inner surface of the upper cap 12 and the lower end cap 13 A ring-shaped sealing pad 17 is provided.

The filter plate 14 installed on the upper cap 12 functions to remove impurities in the organic solvent injected into the extractor body 11 and the filter plate 14 provided on the lower end cap 13 A hard porous ceramic filter having a thin thickness is normally used to finally remove the impurities in the sample liquid discharged through the extraction kit 10 and each filter plate 14 has a function of extracting the sample liquid It is possible to fix the mounting nut 15 to the upper end cap 12 and the lower end cap 13 by using the nut stopper 16 while the mounting nut 15 is manufactured as a separate part.

Therefore, when the filter plate 14 is replaced, the nut stoppers 16 are detached from the stopper mounting grooves 16b of the upper end cap 12 and the lower end cap 13, The nut stopper 16 can be pulled out from the upper end cap 12 or the lower end cap 13 together with the nut stopper 16. In order to more easily perform the separation operation of the nut stopper 16, There is formed a tool insertion hole 16a in which the nut stopper 16 can be elastically pulled out.

3, the sealing pads 17 provided on the mounting nut 15 are fixed to the upper end of the extractor body 11 during the fastening operation of the upper end cap 12 and the lower end cap 13, And the bottom surface of the sample setter 20 is prevented from being in direct contact with the filter plate 14 to prevent damage to the filter plate 14 due to excessive clamping force, So that the organic solvent component and the sample liquid component are prevented from leaking through the assembling portion of the mounting nut 15. The sealing ring 22 is disposed on the side of the filtering plate 14,

According to the present invention having the above-described configuration, it is possible to carry out the operation of injecting several kinds of adsorbents (18) in layers on the upper side of the fiber filter (24) by using the transparent sample inlet tube (21) It is possible to visually check the operation of injecting the sample 19 onto the upper part of the adsorbent layer and the sample sample layer so that the adsorbent layer and the sample sample layer can be set to the precise layered structure according to the required position.

By inserting the sample inlet tube 21 with the sample accurately set in the above manner into the extractor body 11 of the extraction kit 10 together with the buffer seal ring 22, Not only can the extraction operation be performed more quickly and accurately, but also contributes greatly to improving the reliability of the analysis result by optimizing the composition of the extracted sample liquid.

In addition, since the extraction operation of the sample solution by the organic solvent is performed inside the sample setting device 20, it is possible to minimize the contamination occurring in the expensive extraction kit 10 when extracting the sample solution, It is possible to use only the sample setter 20 of a low price and to use it, thereby eliminating the difficult cleaning work of the extraction kit 10 itself and making the economic life of the extraction kit 10 maximized. An extraction method can be provided.

The sample inlet pipe 21 separates the adsorbent 18 treated with strong acidity or strong basicity from the extractor body 11 of the extraction kit 10 so as to increase the removal efficiency of the interference substance. It is possible to prevent the component of the adsorbent 18 from coming into direct contact with the extractor body 11 even when the adsorbent 18 treated with strongly acidic or strong basicity is introduced, It is possible to prevent corrosion of the extraction vessel 10 and to perform a required extraction operation even if the extraction kit 10 dedicated to strong acidity or strong basicity is not separately purchased.

After the extraction of the sample liquid is completed, the upper cap 12 and the lower end cap 13 are separated from the extractor body 11, and then the fiber filter 24 used for the extraction operation is inserted into the sample inlet pipe It is possible to relatively easily determine whether or not the extraction operation is accurate by observing the color of the fiber filter 24 and the extraction path of the sample solution.

Particularly, in a state in which the sample required for the extraction operation is set in advance in the plurality of sample setting devices 20, the sample setting device 20 having been completely extracted is taken out of the extraction kit 10 and then another sample setting device 20 can be immediately mounted on the extraction kit 10 to perform the subsequent extraction operation, so that the extraction operation can be continuously performed several times to several tens of times with only one extraction kit 10.

On the other hand, if the thickness of the sample inlet tube 21 constituting the sample setter 20 of the present invention is made 1 mm and inserted into the extractor body 11 of the extraction kit 10 having a volume of 34 ml, The volume of the extraction kit 10 is automatically adjusted to 22 mL so that the extraction kit 10 of 34 mL can be utilized as the extraction kit 10 of 22 mL volume, It is also possible to prevent an economic burden and a crosstalk in use due to the use of a plurality of such devices.

4 shows a sample setting device 20 according to another embodiment of the present invention. The covering ring 25 covers the upper end surface or the lower end surface of the sample introduction pipe 21, And a mounting ring 26 protruding from the cover ring 25 so as to be inserted into the inner periphery of the upper end of the sample inlet tube 21 or the inner circumferential edge of the lower end of the sample inlet tube 21, The portion of the mounting ring 26 of the cushioning seal ring 22 mounted on the filter support ring 23 functions as the filter support ring 23 and other detailed technical configurations are the same as those of the previously described embodiment .

As described above, according to the sample setting device 20 according to another embodiment of the present invention, the buffering seal ring 22 is directly mounted on the upper and lower ends of the sample introduction pipe 21 to connect the sample setting device 20 to one assembly It is possible to improve the convenience of handling and use of the sample setting device 20 and to improve the convenience of the sample setting device 20 by connecting the two buffer sealing rings 22 and one filter supporting ring 23 to the sample inlet pipe It is possible to provide a simple and practical structure in which the number of parts can be reduced as compared with the case of the embodiment of FIG.

FIG. 5 shows a sample setting device 20 according to another embodiment of the present invention. Referring to FIG. 4, the sample setting device 20 includes an assembly inclined surface 20, And a cover portion 25 of the cushioning seal ring 22 mounted on the upper end side of the sample injection pipe 21 is formed with a sheet portion 21a, which covers the assembly inclined surface 21a of the sample injection pipe 21, And an inner circumferential portion of the buffer seal ring 22 mounted on the lower end of the sample inlet pipe 21 is formed by a funnel-shaped tapered portion 22a.

As described above, according to the sample setting device 20 according to another embodiment of the present invention, the cushioning seal ring 22 provided on the upper surface of the sample injection pipe 21 has the assembly inclined surface 21a and the seat 25a, It is possible to maintain the tight sealing state of the upper side buffer sealing ring 22 by the tightening force of the upper end cap 12 and the injection pressure of the solvent, It is possible to more reliably prevent the leakage of the solvent injected under the sample injection tube 21 and prevent the step portion from being present on the sample solution extraction path on the lower end side of the sample injection tube 21, A sufficient extraction amount can be ensured.

4 and 5, the edge of the covering 25 of the buffer sealing ring 22 mounted on the upper and lower ends of the sample inlet pipe 21 is connected to the inner surface of the extractor body 11 by 0.1 mm or more and a small clearance D in the vicinity of the extractor body 11 so as to insert the sample injection tube 21 equipped with the buffer sealing ring 22 into the extractor body 11 or to take it out of the extractor body 11 It is preferable that the cover ring 25 of the buffer seal ring 22 is not brought into close contact with the inner surface of the extractor body 11.

4 and 5, the sample setting device 20 in a state in which the buffer sealing ring 22 is assembled to the upper and lower sides of the sample introduction pipe 21 is provided in the extractor body 11, The cover ring 25 of the cushioning seal ring 22 is brought into close contact with the inner surface of the extractor body 11 to cause frictional resistance which causes difficulties in performing the operation In addition, there is a possibility that the buffer seal ring 22 may escape from the sample injection tube 21 during the insertion or separation of the sample setting device 20. To prevent such a phenomenon, the cover ring 22 of the buffer seal ring 22 25 are spaced apart from the inner surface of the extractor body 11 by a minute clearance D therebetween.

More preferably, each buffer sealing ring 22 protrudes through the upper and lower ends of the extractor body 11 by a predetermined thickness, preferably about 0.5 mm or less, so that the inside of the extractor body 11 When the upper cap 12 and the lower end cap 13 are fastened together with the sample setting device 20 inserted into the upper end cap 12 and the lower end cap 13 by the fastening force of the upper end cap 12 and the lower end cap 13, It is to be noted that the above-mentioned method is applied to the embodiment described on the basis of FIGS.

1: solvent storage container 1a: solvent supply line 2: mixing valve
3: Infusion pump 3a: Solvent injection line 4: Heating oven
5: Sample storage vessel 5a: Sample extraction line 6: High pressure nitrogen tank
7: relief valve 8: constant pressure valve 10: extraction kit
11: extractor body 11a, 15a: fastening part 12: upper cap
12a: solvent inlet 12b, 13b: recessed portions 12c, 13c: cushioning packing
13: lower cap 13a: sample liquid extraction port 14: filtration plate
15: mounting nut 15b: rotation stopper 15c: rotation preventing groove
16: nut stopper 16a: tool insertion hole 16b: stopper mounting groove
17: sealing pad 18: adsorbent 19: sample sample
20: sample setting device 21: sample introduction pipe 21a: assembly inclined surface
22: buffer sealing ring 22a: tapered portion 23: filter support ring
24: Fiber filter 25: Covering 25a: Sheet portion
26: Mounting ring D: Clearance

Claims (9)

delete delete delete delete An extraction kit 10 for a sample liquid used in an accelerated solvent extraction apparatus includes a cylinder-shaped extractor body 11 for injecting a sample and an upper cap 12 assembled on the upper end of the extractor body 11, And a lower end cap 13 assembled at a lower end of the extractor body 11. A solvent injection port 12a is vertically penetrated through the center of the upper end cap 12, In the extraction kit 10 formed at the center of the cap 13, a sample liquid extraction port 13a is vertically penetrated,
The extraction kit 10 includes a sample setting unit 20 inserted into the extractor body 11 so as to be detachable from the extractor body 11,
The sample setting device 20 includes a cylindrical sample inlet tube 21 made of a transparent material so that the state of the sample can be visually confirmed and the sample setting device 20 disposed at the upper and lower ends of the sample inlet tube 21, A buffer sealing ring 22 for protecting the inlet pipe 21 and preventing leakage of the solvent and the sample liquid and a filter support member 22 mounted on the inner peripheral edge of the lower end of the sample inlet pipe 21 for supporting the fiber filter 24. [ Ring 23,
A mounting nut 15 for fastening assembly of the extractor body 11 is inserted into the upper cap 12 and the lower cap 13 and the upper end of the extractor body 11 and the lower end of the lower end A fastening portion 11a for assembly with the mounting nut 15 is formed,
A rotation preventing jaw 15b is protruded from the outer periphery of the mounting nut 15 and a rotation preventing jaw 15b of the mounting nut 15 is inserted into the inner periphery of the upper cap 12 and the lower end cap 13. [ A rotation preventing groove 15c is formed,
A stopper mounting groove 16b is formed in the lower inner periphery of the upper cap 12 and an upper inner peripheral portion of the lower end cap 13 and a stopper mounting groove 16b is formed in the stopper mounting groove 16b, A nut stopper 16 as a C-shaped elastic frame is fitted,
A filtering plate 14 is disposed on the inner surface of the upper cap 12 corresponding to the outlet of the solvent inlet 12a and the inner surface of the lower cap 13 corresponding to the inlet of the sample liquid extracting aperture 13a, A ring-shaped sealing pad 17 is provided on one side of the mounting nut 15 to closely contact the filtering plate 14 with the inner surface of the upper cap 12 and the lower cap 13,
Wherein a tool insertion hole (16a) is formed on an end side of the nut stopper (16) so that the nut stopper (16) can be retracted using a clamping tool. 6. The apparatus according to claim 5, wherein the buffer seal ring (22) comprises a cover ring (25) covering the upper end surface or the lower end surface portion of the sample injection pipe (21) And a mounting ring (26) which is inserted into the inner periphery of the upper end of the upper end portion (21)
Characterized in that the filter support ring (23) is part of the mounting ring (26) of the cushion seal ring (22) mounted on the lower end of the sample inlet tube (21). The sample injection tube according to claim 6, wherein the upper outer circumferential edge of the sample inlet tube (21) is formed as an assembling slant surface (21a) inclined downward outward, and a buffer sealing ring (22 And a seat part (25a) covering an assembling inclined surface (21a) of the sample introduction pipe (21) is additionally formed on the lower periphery of the cover (25) of the cover (25). The sample setting device according to claim 6, wherein the inner circumference of the buffer seal ring (22) mounted on the lower end of the sample inlet tube (21) is formed of a funnel-shaped tapered portion (22a) Extraction kit. delete
KR20140152571A 2014-11-05 2014-11-05 Extraction kit using setting device of a sample for accelerated solvent extraction KR101507042B1 (en)

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KR101955708B1 (en) 2018-01-04 2019-03-07 주식회사 진시스템 A tube for extracting nucleic acid and method for nucleic acid extraction process using it
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CN112964513A (en) * 2021-04-15 2021-06-15 安徽金种子酒业股份有限公司 Be arranged in tea wine ester material detection device
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KR101421077B1 (en) * 2013-12-11 2014-07-22 대한민국 One-step integrated extraction and cleanup method for analysis of oil contaminants in marine sediments using accelerated solvent extraction

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KR101858358B1 (en) * 2016-10-21 2018-05-15 한국석유관리원 Site monitoring apparatus of oil concentration in soil using solid phase extraction column
KR101955708B1 (en) 2018-01-04 2019-03-07 주식회사 진시스템 A tube for extracting nucleic acid and method for nucleic acid extraction process using it
KR20190142632A (en) * 2018-06-18 2019-12-27 한국원자력연구원 Manufacturing apparatus of planchet sample
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US11050777B2 (en) 2018-11-20 2021-06-29 Saudi Arabian Oil Company Method and system for remediating cybersecurity vulnerabilities based on utilization
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KR102087611B1 (en) * 2019-10-11 2020-03-11 대한민국 One-step integrated extraction and cleanup method for analysis of HBCDs and TBBPA in marine sediments or organism samples using accelerated solvent extractor
CN112964513A (en) * 2021-04-15 2021-06-15 安徽金种子酒业股份有限公司 Be arranged in tea wine ester material detection device
CN114295458A (en) * 2021-12-31 2022-04-08 西安稀有金属材料研究院有限公司 Method for researching in-situ corrosion behavior of metal material at atomic scale
CN114295458B (en) * 2021-12-31 2024-03-19 西安稀有金属材料研究院有限公司 Method for researching in-situ corrosion behavior of metal material by atomic scale

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