JP2005180968A - Collection method and analysis method of residual organic contaminant - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To analyze a residual organic contaminant included in a contaminee polluted by the residual organic contaminant quickly and simply by using an analytical instrument. <P>SOLUTION: This analysis method of a residual organic contaminant includes a process for bringing supercritical fluid such as supercritical carbon dioxide into contact with a contaminee such as soil stored in a cell 21, to thereby acquire an extracted fluid including the residual organic contaminant; a process for allowing the extracted fluid to pass an adsorbent column 3 filled with an adsorbent capable of adsorbing the residual organic contaminant; and a process for heating the adsorbent column 3 after passing of the extracted fluid, and supplying the residual organic contaminant volatilized from the adsorbent to the analytical instrument 4. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for collecting and analyzing persistent organic pollutants, and more particularly to a method for collecting persistent organic pollutants from contaminated materials contaminated with persistent organic pollutants and using the analytical equipment The present invention relates to a method for analyzing residual organic pollutants contained in contaminated materials contaminated with organic pollutants.

  Dioxins such as polychlorinated dibenzo-para-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), polychlorinated biphenyls (PCBs) such as coplanar polychlorinated biphenyls, dichlorodiphenyltrichloroethane (DDT), aldrin, endrin, chlordane, Various organic substances, such as heptachlor, mirex, toxaphene and organochlorine compounds such as hexachlorobenzene, which are not easily decomposed in the environment and have the potential to act as so-called environmental hormones, that is, residual organic pollutants ( POPs: Persistent Organic Pollutants (POPs) are subject to elimination and reduction through international cooperation in the Stockholm Convention (POPs Convention) aimed at protecting human health and protecting the environment. For this reason, persistent organic pollutants include exhaust gas from waste incineration facilities, air, water such as factory effluent and river water, incineration ash such as fly ash generated in waste incineration facilities, soil, etc. It is necessary to periodically analyze the content of

  By the way, when analyzing residual organic pollutants contained in a fluid such as exhaust gas or water or in soil, it is first necessary to collect the residual organic pollutants from a specimen such as exhaust gas or soil. Here, when the specimen is a solid substance such as soil or incinerated ash, an extraction method using a hydrophobic solvent such as toluene or n-hexane from the solid substance, that is, a contaminated substance by a residual organic pollutant. Residual organic pollutants are collected by (for example, Soxhlet extraction method) (see, for example, Non-Patent Documents 1, 2, and 3).

  On the other hand, when the specimen is a fluid such as exhaust gas or water, first, for example, the persistence in the fluid using the glass impinger described in Non-Patent Document 4 or the filters described in Patent Documents 1 and 2 is used. Capture organic pollutants. In this case, the glass impinger or the filter that captures the residual organic pollutant contained in the fluid becomes contaminated by the residual organic pollutant. And the residual organic pollutant of the contaminated material can be collected by an extraction method (for example, Soxhlet extraction method or cleaning method of the contaminated material) using the same hydrophobic solvent as described above (non-patent) Reference 4 and Patent Documents 1 and 2).

  However, these collection methods are uneconomical because they require a large amount of hydrophobic solvent to extract residual organic pollutants from the contaminated material, and are at least several days long for extraction. It takes time.

  In the above-described sampling method, the residual organic pollutant is obtained as an extract with a hydrophobic solvent. Since this extract contains impurities other than the residual organic pollutant, the gas chromatograph mass spectrometer (GC) When analyzing residual organic pollutants using analytical instruments such as / MS), it is complicated and long due to chromatography such as multilayer silica gel column chromatography, activated carbon column chromatography, alumina column chromatography, silica gel chromatography or florisil chromatography, or sulfuric acid treatment. A time-consuming purification process is required. Moreover, it is necessary to concentrate the extract after the purification treatment before supplying it to the analytical instrument.

  An object of the present invention is to efficiently collect a residual organic pollutant in a short time from a contaminated object by the residual organic pollutant.

  Another object of the present invention is to quickly and easily analyze a residual organic pollutant contained in a contaminated material contaminated by the residual organic pollutant using an analytical instrument.

  In the present application, the term dioxins is defined as polychlorinated dibenzo-para-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) following the provisions of Article 2 of the Special Measures Act against Dioxins (1999 Act No. 105). In addition, it is used to mean including coplanar polychlorinated biphenyls (Co-PCBs).

“Soil Survey and Measurement Manual for Dioxins (2000)” edited by Soil Agricultural Chemicals Section, Water Quality Conservation Bureau, Environment Agency "Environmental Agency Water Quality Preservation Bureau Water Quality Management Division" Bottom Quality Survey Manual for Dioxins (2000) " “Environmental Endocrine Disrupting Chemical Substances Interim Manual (1998)” Japanese Industrial Standard JIS K 0311: 1999 established on September 20, 1999

Japanese Patent No. 327396 WO01 / 91883

  The method for collecting persistent organic pollutants according to the present invention is a method for collecting persistent organic pollutants from contaminated materials contaminated with persistent organic pollutants, and contacting the contaminated materials with a supercritical fluid. And obtaining an extraction fluid containing residual organic pollutants and contacting the extraction fluid with an adsorbent capable of adsorbing the residual organic pollutants.

  In this sampling method, when the supercritical fluid is brought into contact with the contaminated material, the residual organic pollutant contained in the contaminated material is efficiently extracted in a short time by the supercritical fluid. A fluid is obtained. Then, when this extraction fluid is brought into contact with an adsorbent capable of adsorbing the residual organic pollutant, the residual organic pollutant contained in the extraction fluid is adsorbed on the adsorbent and collected.

  The method for collecting persistent organic pollutants according to another aspect of the present invention is also a method for collecting the persistent organic pollutants from the contaminated material contaminated by the persistent organic pollutants. The method includes a step of bringing a supercritical fluid into contact with an object to obtain an extraction fluid containing residual organic contaminants, and a step of dissolving the extraction fluid in a solvent.

  In this sampling method, when the supercritical fluid is brought into contact with the contaminated material, the residual organic pollutant contained in the contaminated material is efficiently extracted in a short time by the supercritical fluid. A fluid is obtained. And if this extraction fluid is melt | dissolved in a solvent, a residual organic contaminant will be extract | collected as a solution by the said solvent.

  The method for analyzing residual organic pollutants according to the present invention is a method for analyzing the residual organic pollutants contained in the contaminated material contaminated by the residual organic pollutants using an analytical instrument. Contacting the contaminant with a supercritical fluid to obtain an extraction fluid containing persistent organic contaminants, contacting the extraction fluid with an adsorbent capable of adsorbing the persistent organic contaminants, and contacting the extraction fluid Heating the subsequent adsorbent, and supplying the residual organic pollutants volatilized from the adsorbent to the analytical instrument.

  In this analysis method, when a supercritical fluid is brought into contact with the contaminated material, the residual organic pollutant contained in the contaminated material is efficiently extracted in a short time by the supercritical fluid, and the residual organic pollutant is extracted. A fluid is obtained. When the extraction fluid is brought into contact with an adsorbent capable of adsorbing the residual organic pollutant, the residual organic pollutant contained in the extraction fluid is adsorbed on the adsorbent. Persistent organic pollutants adsorbed on the adsorbent are volatilized when the adsorbent is heated, and can be analyzed by the analytical instrument when volatiles are supplied to the analytical instrument.

  The analysis method for persistent organic pollutants according to the present invention is also a method for analyzing the residual organic pollutants contained in the contaminated material contaminated with the persistent organic pollutants using an analytical instrument. A step of contacting a contaminated material with a supercritical fluid to obtain an extraction fluid containing persistent organic pollutants; a step of dissolving the extraction fluid in a solvent to prepare a solution of persistent organic pollutants; and A step of bringing the solution into contact with an adsorbent capable of adsorbing contaminants, and a step of heating the adsorbent after contacting the solution and supplying residual organic contaminants volatilized from the adsorbent to the analytical instrument. Including.

  In this analysis method, when a supercritical fluid is brought into contact with the contaminated material, the residual organic pollutant contained in the contaminated material is efficiently extracted in a short time by the supercritical fluid, and the residual organic pollutant is extracted. A fluid is obtained. After this extraction fluid is dissolved in a solvent to prepare a solution of persistent organic pollutants, the solution is brought into contact with an adsorbent capable of adsorbing the residual organic contaminants. The substance adsorbs on the adsorbent. Persistent organic pollutants adsorbed on the adsorbent are volatilized when the adsorbent is heated, and can be analyzed by the analytical instrument when volatiles are supplied to the analytical instrument.

  Since the method for collecting persistent organic pollutants according to the present invention includes the steps as described above, the residual organic pollutants are efficiently collected in a short time from the contamination by the persistent organic pollutants. be able to.

  Since the method for analyzing persistent organic pollutants according to the present invention includes the steps as described above, the residual organic pollutants contained in the contaminated material contaminated by the persistent organic pollutants are analyzed using an analytical instrument. It can be used for quick and simple analysis.

Form 1
With reference to FIG. 1, one form of the analyzer for implementing simultaneously the collection method and analysis method of the persistent organic pollutant which concern on this invention is demonstrated. In the figure, the analysis device 1 mainly includes an extraction unit 2, an adsorbent column 3, and an analysis device 4.

  The extraction unit 2 is for extracting the residual organic pollutant from the contaminated material contaminated by the persistent organic pollutant, and supplies the cell 21, the oven 22 and the carbon dioxide for containing the contaminated material. The apparatus 23 and the back pressure regulator 24 are mainly provided. The oven 22 is for heating the cell 21 and a part of a gas supply path 26 described later. The cell 21 is accommodated in the oven 22.

  The supply device 23 mainly includes a gas cylinder 25 for carbon dioxide and a gas supply path 26. The gas supply path 26 extends from the gas cylinder 25, and includes a cooler 27 for cooling the carbon dioxide gas from the gas cylinder 25 side, a pump 28 for supplying the carbon dioxide gas into the cell 21 while being pressurized, and an injector 29. Are provided in this order. The gas supply path 26 is connected to the lower part of the cell 21 housed in the oven 22. The injector 29 is for injecting an entrainer for accelerating the extraction of the residual organic pollutant from the contaminated material into the carbon dioxide gas supplied into the cell 21. 50 and an injection path 52 having a pump 51 that extends from the storage tank 50 and is connected to the gas supply path 26. The entrainer used here is, for example, water or an organic solvent such as methanol, ethanol, acetone, hexane, toluene, dichloromethane, dimethyl sulfoxide, or acetonitrile. Two or more of these entrainers may be used as a mixture.

  In the supply device 23 described above, the oven 22 and the pump 28 are capable of heating and pressurizing the carbon dioxide, respectively, so that the carbon dioxide from the gas cylinder 25 is converted into supercritical carbon dioxide (an example of a supercritical fluid). have.

  The back pressure regulator 24 is connected to a first communication path 53 extending from the upper part of the cell 21, and is used to depressurize supercritical carbon dioxide from the first communication path 53 and release the supercritical state. is there.

  The adsorbent column 3 has a cylindrical body that opens in the vertical direction and is filled with the adsorbent, and a second communication path 54 extending from the back pressure regulator 24 is connected to the upper end. Further, the adsorbent column 3 includes a heater 31 for heating. The adsorbent used in the adsorbent column 3 is not particularly limited as long as it can adsorb residual organic pollutants, and examples thereof include silica gel-based, carbon-based, alumina-based and florisil-based materials. Can do. These adsorbents are appropriately subjected to surface structure processing and functional group addition in order to enhance the specific adsorptivity of persistent organic pollutants and to suppress the adsorption of substances other than persistent organic pollutants. May be. Moreover, these adsorbents can also be used in a mixture of two or more.

  However, the adsorbent used here is a fiber material (a group of fiber materials) and an inorganic binder because it is easy to handle and the adsorbed residual organic pollutants are easily desorbed by the heating process described later. In particular, those having a three-dimensional network structure having fluid permeability are preferable. The fiber material used in this molded body does not substantially react chemically with the residual organic pollutant, and is usually fibrous activated carbon, carbon fiber, glass fiber, alumina fiber (preferably activated alumina fiber), silica fiber. And at least one of fluororesin fibers (for example, Teflon fiber: Teflon is a registered trademark). On the other hand, an inorganic binder is a material that binds fiber materials together to integrate a group of fiber materials, and has a property of imparting a fixed shape to the group of fiber materials, that is, a group of fiber materials. It functions as a binder that maintains a fixed molding shape.

  The inorganic binder that can be used here is not particularly limited as long as it has the above-described performance and does not substantially chemically react with the residual organic pollutant like the fiber material. Those having performance, particularly adsorption performance for persistent organic pollutants are preferred. Examples of such inorganic binders include alumina (preferably activated alumina), zeolite (preferably synthetic zeolite), silicon dioxide (silica), acid clay, apatite, and the like. The materials may be used alone or in combination of two or more. Further, the form of the inorganic binder is not particularly limited, but usually a particulate one is used.

  It is preferable that the above-mentioned molded body is usually set to a bulk density that allows an extraction fluid described later to pass smoothly.

  An example of a method for producing such a molded body is described in, for example, WO 01/91883 (the above-mentioned Patent Document 2). Incidentally, as such a molded body, for example, “Dioana” of Miura Kogyo Co., Ltd. (“Dioana” is a registered trademark of Miura Kogyo Co., Ltd.) can be used.

  The analytical instrument 4 is capable of qualitatively and quantitatively analyzing residual organic pollutants, and is, for example, various gas chromatograph mass spectrometers (GC / MS). The analytical instrument 4 has an introduction port 41 for introducing a sample to be analyzed, and a third communication path 55 extending from the lower part of the adsorbent column 3 communicates with the introduction port 41. The third communication path 55 has a switching valve 56. The switching valve 56 communicates with a discharge path 57 for discharging the fluid generated in the back pressure regulator 24 and passed through the adsorption column 3, and communicates between the adsorbent column 3 and the introduction port 41 or the adsorbent column. 3 is a three-way valve for switching the third communication path 55 to any one of the communication between the discharge path 57 and the discharge path 57.

  Next, a method for analyzing residual organic contaminants using the above-described analyzer 1 will be described. In the analyzer 1, the switching valve 56 is set in advance so that the adsorbent column 3 and the discharge path 57 communicate with each other.

  First, the contaminated material contaminated with the residual organic pollutant is accommodated in the cell 21. Here, the contaminated material is not particularly limited as long as it is a solid substance contaminated with persistent organic pollutants. For example, in soil contaminated with persistent organic pollutants, waste incineration facilities Captured and collected residual organic pollutants contained in incineration ash such as generated fly ash and furnace bottom ash, exhaust gas from waste incineration facilities, and wastewater discharged from various factories such as paper mills Examples include filters (for example, those described in Patent Documents 1 and 2 above).

  Next, the oven 22 is heated, and carbon dioxide is supplied from the gas cylinder 25 to the gas supply path 26. The carbon dioxide supplied to the gas supply path 26 is cooled in the cooler 27 and is continuously supplied into the cell 21 while being pressurized by the pump 28 and heated in the oven 22. At this time, the pump 51 is also operated, and the entrainer in the storage tank 50 is injected into the carbon dioxide being supplied to the cell 21 through the injection path 52.

  The carbon dioxide supplied into the cell 21 becomes supercritical carbon dioxide, and comes into contact with the contaminated material accommodated in the cell 21. As a result, the residual organic pollutant contained in the contaminated material is efficiently extracted in a short time by supercritical carbon dioxide. At this time, since supercritical carbon dioxide includes an entrainer, the residual organic pollutant is more efficiently extracted from the contaminated material. Then, the supercritical carbon dioxide from which the residual organic pollutants are extracted is supplied from the cell 21 to the back pressure regulator 24 through the first communication path 53 and is depressurized there. As a result, the supercritical carbon dioxide extracted from the residual organic pollutant is separated into a gas phase and a liquid phase, and an extraction fluid for the residual organic pollutant is obtained.

  The obtained extracted fluid is supplied from the back pressure regulator 24 to the adsorbent column 3 through the second communication path 54. Here, the residual organic contaminant contained in the extraction fluid is adsorbed by the adsorbent filled in the adsorbent column 3. As a result, the residual organic pollutant is separated from the extraction fluid and collected in the adsorbent of the adsorbent column 3. On the other hand, the extracted fluid after the residual organic pollutant is separated passes through the adsorbent column 3 and is discharged to the outside from the discharge path 57.

  Next, after switching the switching valve 56 so that the adsorbent column 3 and the introduction port 41 communicate with each other, the heater 31 for heating is operated again. Thereby, the adsorbent column 3 is heated and the residual organic pollutant collected by the adsorbent volatilizes. Then, the volatilized residual organic pollutant is supplied to the introduction port 41 through the third communication path 55 and analyzed by the analysis device 4.

  As described above, this analysis method uses supercritical carbon dioxide to extract persistent organic pollutants from contaminated materials. Can be efficiently collected. In addition, this sampling step does not require the use of an organic solvent substantially, or the amount of the organic solvent used can be suppressed to a very small amount compared to the conventional method using the Soxhlet extraction method. There is little risk of work environment pollution or environmental pollution. Furthermore, in this analysis method, since the residual organic pollutant collected in the adsorbent is heated and volatilized by the heater 31 for heating, the collected residual organic contamination is not subjected to complicated purification processing and concentration processing. Substances can be analyzed quickly and simply by the analytical instrument 4.

Form 2
With reference to FIG. 2, one form of the collection device for implementing the collection method of the persistent organic pollutant which concerns on this invention is demonstrated. In the figure, the collection device 100 is for collecting the residual organic pollutant from the contaminated material by the residual organic pollutant, and mainly includes the extraction unit 2 and the solvent container 110.

  The extraction unit 2 is configured in the same manner as the extraction unit 2 of the analyzer 1 according to the first embodiment described above. In FIG. 2, the same parts as those in FIG. On the other hand, the solvent container 110 stores the solvent 111, and the tip of the discharge path 112 extending from the back pressure regulator 24 is disposed in the solvent 111. The solvent 111 stored in the solvent container 110 is not particularly limited as long as it can dissolve residual organic pollutants, but usually acetone, toluene, hexane, methanol, ethanol, dichloromethane, dimethyl sulfoxide, acetonitrile , An organic solvent such as decane or nonane, or water. Two or more kinds of these solvents may be used in combination as appropriate.

Next, a method for collecting persistent organic contaminants using the above-described collection device 100 will be described.
First, the contaminated material contaminated with the residual organic pollutant (similar to the contaminated material in the first embodiment described above) is accommodated in the cell 21. And it operates similarly to the case of the above-mentioned form 1, and the extraction fluid is obtained in the back pressure regulator 24.

  The obtained extracted fluid moves through the discharge path 112 and is ejected into the solvent 111 stored in the solvent container 110. Thereby, the extraction fluid is dissolved in the solvent, and the residual organic contaminant contained in the extraction fluid is collected as a solution dissolved in the solvent 111.

  As described above, this sampling method uses supercritical carbon dioxide to extract persistent organic pollutants from the contaminated material. Organic pollutants can be collected. Further, this sampling method can suppress the amount of organic solvent used to a small amount as compared with the conventional method using the Soxhlet extraction method, and therefore there is less risk of work environment contamination and environmental contamination by volatile solvents.

Next, a method for analyzing residual organic pollutants using the above sampling method will be described.
First, the solution of the residual organic pollutant obtained according to the above sampling method is brought into contact with the adsorbent, and the residual organic pollutant in the solution is adsorbed onto the adsorbent. Here, usually, an adsorbent is packed in a column, and the solution is passed through the column. At this time, the solution is preferably concentrated in advance. The adsorbent used here is not particularly limited as long as it can adsorb persistent organic pollutants, and is usually the same as that used in the adsorbent column 3 of the above-described embodiment 1. .

  Next, an analytical instrument capable of qualitatively and quantitatively analyzing residual organic pollutants, for example, a connecting tube between the introduction port of various gas chromatograph mass spectrometers (GC / MS) and one end of the above-mentioned column is used. Connect and heat the column. As a result, the adsorbent is heated and the residual organic pollutant adsorbed on the adsorbent volatilizes. The volatilized residual organic pollutant is supplied to the introduction port of the analytical instrument through the connecting pipe and analyzed by the analytical instrument.

  As described above, this analysis method is obtained by the above sampling method because the residual organic pollutant adsorbed on the adsorbent is volatilized by heating the adsorbent and supplied to the analytical instrument through the connecting tube. Thus, residual organic pollutants can be analyzed quickly and easily with an analytical instrument without purifying and concentrating the solution.

[Other embodiments]
(1) In each of the above embodiments, supercritical carbon dioxide is used as a supercritical fluid. However, the present invention is similarly implemented when a supercritical fluid other than supercritical carbon dioxide, for example, supercritical nitrous oxide is used. can do.

(2) The analysis method in the above-described embodiment 2 is for injecting an analysis sample into an introduction port equipped with an analysis device such as GC / MS and having a function for heating and vaporizing the sample. An injector equipped with an adsorbent capable of adsorbing a sample can also be used. In this case, the solution obtained by the above-described sampling method is appropriately concentrated and sucked into the injector, and the residual organic contaminant contained in the solution is adsorbed on the adsorbent in the injector. When the injector is inserted into the introduction port of the analytical instrument, the introduction port heats the injector and volatilizes the residual organic contaminants adsorbed on the adsorbent. Then, the volatilized residual organic pollutant is supplied in this state into the introduction port and analyzed by the analytical instrument.

  Examples of the injector as described above include a solid-phase microextraction injector (SPME) manufactured by Spelco, Inc., sold through Sigma-Aldrich Japan, Inc., Scientific Instrument Services Inc. The product name “Short Path Thermal Deposition Model TD-4” of the company and the product name “TDS A, TDS 2, CIS 4” which is a heat desorption introduction system manufactured by Gerstel can be used.

Comparative Example A paddy soil in the Matsuyama Plain, Ehime Prefecture, contaminated with dioxins derived from past agricultural chemicals was collected as a contaminated material. Then, dioxins contained in 5 g of the contaminated material were extracted, and 11 kinds of substances shown in Table 1 which are main isomers were qualitatively and quantitatively analyzed. Here, extraction and analysis of dioxins from contaminated materials are described in “Soil Survey and Measurement Manual for Dioxins (2000)” edited by the Environment Agency Water Quality Conservation Bureau Soil Agricultural Chemicals Section (2000). Performed according to the method. At this time, the time required from the start of extraction to the completion of analysis was 4 days. The results are shown in Table 1.

Example 5 g of the same paddy field soil collected in the comparative example was prepared as a contaminated material. And after adding the internal standard substance (cleanup spike) of PCDDs and PCDFs to this to-be-contaminated thing, dioxins were extract | collected from this to-be-contaminated object using the sampling device 100 concerning the above-mentioned form 2. Here, in the cell 21, supercritical carbon dioxide was generated at a pressure of 30 MPa, a temperature of 130 ° C., and a flow rate of 2 ml / min, and dioxins were extracted from the contaminated substances. In this extraction, water was injected at a rate of 2% as an entrainer with respect to the flow rate of carbon dioxide supplied from the injector 29 to the cell 21. Moreover, the extraction fluid from the back pressure regulator 24 was ejected in 150 ml of hexane stored in the solvent container 110 to collect dioxins. The time required for collecting dioxins was about 50 minutes.

  Next, using a rotary evaporator, the hexane solution of dioxins obtained in the above-described collection step was concentrated, and nonane was added thereto to prepare a 0.1 ml solution. This nonane solution was sucked by a sample injector for GC / MS (SPME manufactured by Spellco) equipped with an adsorbent, and dioxins were adsorbed on the adsorbent. In addition, the sample injector used what coated the carbon type adsorbent (Carboxen / PDMS) to the fiber as an adsorbent.

  Next, among the dioxins adsorbed on the adsorbent of the sample injector, 11 kinds of substances to be analyzed in the comparative example were qualitatively and quantitatively analyzed using high resolution GC / MS. Here, the above-mentioned sample injector is attached to the high-resolution GC / MS introduction port, the adsorbent of the sample injector is heated, and dioxins adsorbed on the adsorbent are volatilized for high-resolution GC / MS analysis. The column was fed. For high resolution GC / MS, the product name “JMS-700D” of JEOL was used, and for the analysis column, the product name “DB-5MS” of J & W Scientific was used. The results are shown in Table 1. The time required from the start of collecting dioxins from the contaminated material to the completion of the analysis was 3 hours in total.

  According to Table 1, it turns out that the analysis result in an Example is substantially the same as the analysis result of a comparative example about each isomer of dioxins. From this, it can be seen that the analysis method of the example has the same reliability as the analysis method of the comparative example.

BRIEF DESCRIPTION OF THE DRAWINGS Schematic of an example of the analyzer which can implement simultaneously the collection method and analysis method of the persistent organic pollutant which concern on this invention. Schematic of an example of the collection device which can implement the collection method of the persistent organic pollutant concerning the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Analyzer 2 Extraction part 3 Adsorbent column 4 Analytical instrument 100 Sampling device 111 Solvent

Claims (4)

A method for collecting said persistent organic pollutant from a contaminated material contaminated by persistent organic pollutant,
Contacting a supercritical fluid with the contaminated material to obtain an extraction fluid containing the persistent organic contaminant;
Contacting the extraction fluid with an adsorbent capable of adsorbing the residual organic contaminants;
For collecting persistent organic pollutants including A method for collecting said persistent organic pollutant from a contaminated material contaminated by persistent organic pollutant,
Contacting a supercritical fluid with the contaminated material to obtain an extraction fluid containing the persistent organic contaminant;
Dissolving the extraction fluid in a solvent;
For collecting persistent organic pollutants including A method for analyzing the residual organic pollutant contained in the contaminated material contaminated with the residual organic pollutant using an analytical instrument,
Contacting a supercritical fluid with the contaminated material to obtain an extraction fluid containing the persistent organic contaminant;
Contacting the extraction fluid with an adsorbent capable of adsorbing the residual organic contaminants;
Heating the adsorbent after contacting the extraction fluid and supplying the residual organic contaminants volatilized from the adsorbent to the analytical instrument;
For analysis of persistent organic pollutants including A method for analyzing the residual organic pollutant contained in the contaminated material contaminated with the residual organic pollutant using an analytical instrument,
Contacting a supercritical fluid with the contaminated material to obtain an extraction fluid containing the persistent organic contaminant;
Dissolving the extraction fluid in a solvent to prepare a solution of the persistent organic contaminant;
Contacting the solution with an adsorbent capable of adsorbing the residual organic contaminants;
Heating the adsorbent after contacting the solution and supplying the residual organic contaminants volatilized from the adsorbent to the analytical instrument;
For analysis of persistent organic pollutants including

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