JP2006084440A - Released gas exhausting device, and released gas collecting method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a highly sensitive and highly accurate evaluation device and method in evaluation of a polar compound released from a sample. <P>SOLUTION: A housing container 2 is made of vitreous carbon, the sample 1 is installed in the housing container 2, carrier gas is introduced into the housing container 2, the carrier gas is exhausted from the housing container 2, and the polar compound diffused from the sample 1 in emission gas is measured. The sample 1 is taken out of the housing container 2, the housing container 2 is heated, and a residual polar compound adsorbed to a container inner face is released and measured. By the method, highly sensitive and highly accurate measurement of the polar compound released from the sample 1 becomes possible. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a diffused gas discharge device and a diffused gas collection method.

  In the development of cutting-edge semiconductor elements in recent years, there is an increasing need to reduce contamination in the manufacturing environment and storage environment of semiconductor elements. For this reason, for example, it is important to measure components of chemical substances that remain in a clean room or a building such as a residence or are diffused into the air over time.

  For example, after collecting gas released from building materials (hereinafter referred to as emitted gas) and evaluating organic compounds, etc. in the emitted gas, after installing building members in the container and introducing clean gas into the container A method is known in which a container is heated at a predetermined temperature, and a gas emitted from a sample is collected and measured.

  For example, in Patent Document 1, an organic compound adsorbed by heating the sample at a high temperature in a furnace is diffused from the sample, further concentrated in a trap tube for collecting the emitted gas, and adsorbed on the trap tube by heating the trap tube. A method for desorbing organic compounds is disclosed.

  As described above, a container made of stainless steel, glass, quartz or the like has been conventionally used as a container for storing a sample to be analyzed (hereinafter referred to as a storage container). However, in the case of a storage container using such a material, there is a problem that a part of the emitted gas component, particularly a polar compound, is adsorbed on the inner surface of the storage container or the like.

Further, when heating is performed for desorption of the diffused gas adsorbed on the inner surface of the storage container (hereinafter referred to as thermal desorption), for example, when a conventional storage container using quartz or the like is used, the adsorbed diffused gas is heated. May denature and make measurement difficult. In particular, in the case of performing a very small amount of analysis, there is a problem that the analysis result is greatly reduced due to the fact that the evolved gas is adsorbed on the surface of the storage container or is denatured by heating, and the analysis result is greatly affected. It was.
JP 2000-187027 A

  An object of the present invention is to provide a diffused gas discharge device and a diffused gas collection method that are suitable for use in microanalysis or the like for measuring a diffused gas from a sample and that have a small amount of diffused gas remaining in a storage container.

  In order to achieve the above-mentioned object, a diffused gas discharge apparatus according to the present invention has a discharge port that communicates with a collecting agent, a glassy carbon storage container for storing a sample, and a diffused gas diffused from the sample as described above. It has a discharge means for discharging from the discharge port, and a heating means for heating the storage container after taking out the sample.

  Further, the emitted gas from the sample is preferably a polar compound.

  The method for collecting a diffused gas according to the present invention includes a step of diffusing volatile diffused gas from a sample stored in a glassy carbon storage container, a step of discharging the diffused gas in the storage container, and a discharge Collecting the emitted gas, heating the storage container from which the sample has been taken out, discharging the residual gas remaining on the inner surface of the storage container, and collecting the discharged residual gas And a step of performing.

  Moreover, it is preferable that the said emitted gas is a polar compound.

  According to the present invention, it is possible to provide a diffused gas discharge apparatus and a diffused gas collection method that are suitable for use in microanalysis for measuring a diffused gas from a sample and that have a small amount of diffused gas remaining in a storage container.

  The present inventors have realized that desorption is easy even when a diffused gas from a sample, particularly a diffused gas containing a polar compound, is adsorbed on the glassy carbon surface, and the present invention has been achieved.

  Hereinafter, an apparatus for discharging a diffused gas from a sample will be described with reference to FIG.

  For example, an exhaust gas exhausting apparatus uses a building member as a sample 1, a storage container 2 for storing the sample 1, a heating device 3 for adjusting the temperature of the storage container 2, and a carrier for promoting the recovery of the diffused gas. A gas inlet 4 for introducing gas, a gas outlet 5 for discharging the carrier gas from the storage container 2, and a collector 6 for collecting the emitted gas from the discharged carrier gas are provided. A collection pipe 7, a pump 8 for sucking a gas such as a carrier gas and a diffused gas existing in the storage container 2, and an integrating flow meter 9 for measuring the total amount of a gas such as a carrier gas discharged from the storage container 2. Consists of.

  In the present embodiment, the storage container 2 uses glassy carbon. The glassy carbon has excellent characteristics in that when the emitted gas is thermally desorbed from the storage container 2, the emitted gas is difficult to be chemically adsorbed on the inner surface of the storage container 2. The difficulty of adsorbing the diffused gas on the inner surface of the storage container 2 is suitable for performing a microanalysis because the amount of the diffused gas that may be denatured during thermal desorption decreases.

  The glassy carbon used for the storage container 2 preferably has a surface roughness (Ra) of 0.1 μm or less. Since the storage container 2 is heated and desorbs the emitted gas as will be described later, by providing the inner surface of the storage container with a smoothness (Ra) of 0.1 μm or less, the thermal desorption of the emitted gas can be achieved. improves. In addition, the storage container may be cleaned in the process of measuring the gas emitted from the sample. Therefore, the inside of the container has a level surface with no irregularities, which improves operability and is preferable. . Moreover, it is preferable that an outer periphery is a shape which is easy to contact the inner surface of the heating apparatus 3.

  Although the capacity | capacitance of a storage container is not specifically limited, For example, when putting the sample piece of 30 cm in length and 30 cm in width, it is preferable to use a storage container with a capacity | capacitance of 100-200L. When used in this size, a gas such as a diffused gas or a carrier gas can be circulated, and the sample can be placed in a state where the internal gas can be mixed. As a result, the emitted gas can be sufficiently discharged. For example, in the case of a small sample of about 2 cm square, it is possible to use a storage container having a capacity of 10 to 30 mL.

  Further, when the thickness of the storage container is 1 mm to 10 mm, preferably 2 mm to 5 mm, the container is not easily damaged and the operability as the storage container is good. Is preferable because of shortening. Moreover, not only when the material of the container itself is only glassy carbon, but also by using a container using a refractory having a fire resistance of 1000 ° C. to 1200 ° C. and covering the inner surface with glassy carbon. It can be applied to trace element amount analysis.

Examples of the refractory include nitrides such as Si ₃ N ₄ , AlN, BN, TaN, and NbN, carbides such as TaC, HfC, TiC, WC, SiC, and B ₄ C, W ₂ B, and Mo ₃ B. ₂ , borides such as ZrB ₂ , TiB ₂ , HfB ₂ , TaB ₂ , oxides such as SiO ₂ , Al ₂ O ₃ , ZrO ₂ , MoSI ₂ , WSi ₂ , Zr ₃ Si ₃ , Ta ₅ Si ₃ The glassy carbon raw material is applied to the inner surface of the container formed into a three-dimensional container with a silicide such as the above, and fired in an inert gas, or the glassy carbon is sputtered on the surface of the three-dimensional container. It can be used as a container for microanalysis, for example, by coating.

  Moreover, it is preferable that the inlet and the outlet for introducing the carrier gas have a shape that can be easily connected to other equipment.

  The heating device 3 is a device for heating in order to thermally desorb the diffused gas adsorbed in the storage container, and is a constant temperature bath capable of maintaining a temperature required for volatilization of the diffused gas, a temperature of about 200 to 500 ° C. Etc. are preferably used. As will be described later, when the container is cleaned by heating, the heating device 3 may be used.

  The carrier gas is a gas for facilitating the collection of the gas diffused from the sample (radiated gas), and any gas having low adsorptivity to the storage container etc. may be used, but helium gas, nitrogen gas, and It is preferred to use high purity air. In particular, helium gas or nitrogen gas is preferably used because oxygen contained in the air may oxidize components of the gas to be analyzed during high-temperature heating.

  The collection agent 6 for collecting the emitted gas is, for example, a porous body capable of adsorbing a gaseous substance, such as Tenax (registered trademark) TA, porous polymer, graphite carbon, and carbon molecular sieve. It can be used, and several of these may be used by being filled in multiple layers.

  The collection tube 7 filled with the collection agent only needs to have heat resistance in the operating temperature range of about 300 ° C. to 400 ° C., and for example, glass, stainless steel or the like can be used. Instead of the collection tube, it can be collected by a filter holder, a cartridge type, or a collection tube having an adsorbent inside.

  The pump 8 which is a means for discharging the gas in the storage container such as the carrier gas and the diffused gas may be any pump that can draw a predetermined amount of gas at a predetermined suction pressure, and measures the total amount of the carrier gas and the like. The integrating flow meter 9 may be any as long as it has a range in which a predetermined flow rate can be measured.

  Next, a collection method in the case of using a diffused gas discharge device will be described.

  First, in order to reduce the components of the emitted gas to be analyzed as much as possible and improve the accuracy of the analysis, the storage container or the collection tube provided with the collection agent is washed. Cleaning is performed by heating (hereinafter referred to as heat cleaning), and is performed according to the following procedure.

  First, in a state where high purity helium gas is introduced into a storage container or a collection tube, the container is heated in a range of 200 ° C. to 500 ° C., preferably 300 ° C. to 400 ° C. for 3 to 4 hours. As a result, impurities adhering to the storage container before use are desorbed, and mixing of impurities during collection of the diffused gas is reduced. Thereafter, the storage container or the collection tube is cooled to room temperature. Introduce high-purity air as a carrier gas into the storage container or collection tube, and determine whether any components that affect the analysis remain in the discharged carrier gas, and the concentration before starting the analysis (hereinafter referred to as background) taking measurement. When the background of the substance to be analyzed is sufficiently lower than the concentration evaluated by analysis, it can be used for the analysis operation using a heat-cleaned storage container or collection tube.

  On the other hand, if the concentration is higher than the concentration evaluated by analysis, it is further washed as follows.

  First, the storage container or the collection tube is immersed in a mixed solution of sulfuric acid and hydrogen peroxide solution. Thereafter, the storage container or the collection tube is immersed in pure water and subjected to ultrasonic cleaning. The sulfuric acid used for this washing may be performed using nitric acid or hydrochloric acid.

  Next, the storage container or the collection tube is washed with methanol and acetone. As the organic solvent used for this washing, hexane, dichloromethane, acetonitrile, tetrahydrofuran or the like can be used.

  After that, it is washed again by heating, the background is measured as described above, and it is used after confirming whether the background of the substance to be analyzed is sufficiently lower than the concentration evaluated by the analysis.

  When the container or the collecting tube is not used immediately after washing, it is preferably stored in a desiccator containing activated carbon.

  In order to collect the emitted gas, it is preferable that the collecting agent accommodated in the collecting tube is also heated and washed. For example, in the case of TENAX (registered trademark) TA, heat washing is performed at 250 ° C. to 300 ° C., preferably 280 ° C. for 4 to 6 hours, preferably 5 hours, and the background is confirmed in the same manner as the storage container or the collection tube.

  The emission gas is generally collected at a room temperature of 27 to 29 ° C. and is collected at a relative humidity of 45% to 55%. Details of the collection method are as follows.

  For example, when a piece of building material is used as a sample and the gas emitted from the sample is collected at room temperature, the sample is first placed in a storage container and sealed with a lid. A storage container containing a sample is placed in an apparatus such as a dry bath, and a carrier gas, for example, high-purity air is introduced from a gas inlet while adjusting the temperature to room temperature (27 ° C. to 29 ° C.).

  In order to obtain the gas diffused from one piece of sample, it is preferable to flow 3 to 3.5 liters of carrier gas into the storage container, and high purity at a flow rate of 50 to 60 ml per minute for 5 to 6 minutes. Allow air to circulate.

  The collection tube containing the collection agent is connected to the gas outlet of the storage container, and collects the gas released from the sample.

  Thereafter, the sample is taken out of the storage container, and the carrier gas is changed to an inert gas, for example, high-purity helium gas. When heating the storage container, which will be described later, if the high-purity air remains, the emitted gas may be oxidized. Therefore, the carrier gas is preferably changed from the high-purity air to an inert gas. At this time, the collection tube may be replaced with a new collection tube containing a new collection agent.

  In order to desorb the components of the diffused gas adsorbed on the surface of the storage container (residual gas of the diffused gas), make sure that the container is sealed again, and that the collection tube is attached. Introduce into the storage container.

  The temperature of the dry bath should be heated to 300-400 ° C., the temperature required for desorption of the diffused gas, and 3 to 3.5 liters of gas should be circulated, with a flow rate of 50 ml to 60 ml per minute inside the storage container. For 5 to 6 minutes. The helium gas used as the carrier gas may be replaced with nitrogen gas.

  After circulating a predetermined amount of high-purity helium gas into the storage container, the collection tube is removed.

  The removed collection tube is measured using a measurement device with a heat desorption device, for example, a gas chromatography mass spectrometer (hereinafter referred to as GC / MS).

  In such a procedure, gas (emission gas) emitted from the sample is collected, and the components of the emission gas are measured.

  In particular, in the process of taking a sample from a storage container and heating the storage container at a predetermined temperature, in the conventional storage container, the problem is that particularly polar compounds in the emitted gas are chemically adsorbed on the surface (inner surface) of the storage container. was there. Further, when these polar compounds are adsorbed on the surface of the storage container, they may remain on the surface of the storage container even if they are heated at a temperature necessary to desorb the nonpolar compound. When the storage container formed of glassy carbon shown in the present embodiment is used, components of the emitted gas, particularly polar compounds, are not chemically adsorbed on the surface of the storage container, and even nonpolar compounds can be easily desorbed. Therefore, it is difficult to remain on the surface of the storage container. Therefore, if a storage container using glassy carbon is used as a storage container for measuring the emitted gas from the sample, it is possible to perform highly accurate analysis.

  Further, the sample used in the emission gas discharge device and the emission gas collection method described in the present embodiment is not particularly limited, but the manufacturing apparatus for the electronic industry and its members, the conveyance device for the electronic industry and its members, and the building material. And housing equipment members, furniture, textile products, and resin molded products.

  Examples of the building material include wall materials, floor materials, ceiling materials, partition panels, sealing materials, caulking materials, filters, ducts, tiles, tatami mats, fittings, adhesives, heat insulating materials, soundproof materials, paints, and the like. In particular, as building materials for clean rooms, members such as wall materials, floor materials, ceiling materials, partition panels, sealing materials, caulking materials, filters, fan filter units, piping, ducts, adhesives, and paints can be cited.

  Examples of the manufacturing apparatus for the electronic industry include an exposure apparatus, a CVD apparatus, and a diffusion apparatus. Examples of the member include members such as a housing, an electric circuit board, wiring, piping, and a motor. Examples of the transport device for the electronics industry include a wafer carrier case and a transport robot. Examples of the member include members such as a wafer carrier case and a wafer cassette.

  Examples of the housing equipment member include a system kitchen, a unit bath, a vanity, a blind, an accordion curtain, and a partition. Examples of the furniture include a storage device such as a chest cabinet, a desk, a table, and a chair.

Examples of the textile product include clothing, curtains, and carpets. Examples of the resin molded product include wallpaper, table cloth, toys, baby bottles, tableware, food containers, food packaging materials, and automobile interior materials.

  An example in which the measurement of the diffused gas by the diffused gas discharge device using the storage container formed of glassy carbon shown in the present embodiment is evaluated is shown below.

  In order to evaluate the easiness of desorption to the storage container, the following tests were conducted in order to measure the residual rate of the emitted gas of the polar compound in the gas emitted from the sample to the discharge device.

(Experiment 1)
As typical examples of polar compounds, acetophenone, myristic acid, dodecanal, di-2-ethylhexyl adipate, dibutyl phthalate (BHT), triphenyl phosphate, di-2-ethylhexyl phthalate (DOP) standard substances (hereinafter simply referred to as “DOP”) These standard substances were added to the storage container and the released gas was collected by the following method, and the residual rate on the surface of the storage container was measured.

  The storage container used is made of glassy carbon having a surface roughness Ra = 0.1 μm or less. The storage container had a capacity of 30 mL, the inside of the storage container was smooth, and the thickness of the glassy carbon at the bottom of the storage container in contact with the heating device was 3 mm.

  The emission device for the emission gas includes a glassy carbon storage container, a dry bath for adjusting the temperature of the storage container, a collection tube having a collection agent for collecting the emitted emission gas, It consists of a pump for sucking a gas such as a carrier gas and a diffused gas existing in the storage container, and an integrating flow meter for measuring the total amount of the carrier gas that flows into and out of the sample.

  First, the storage container formed of glassy carbon is cleaned. Washing is performed by heating and washing as follows.

  Installed in dry bath with high purity helium gas introduced into the storage container and heated at 350 ° C. for 3 hours. Then, it is cooled to room temperature, and the background is measured by changing the carrier gas to high-purity air. After confirming that the background of the polar compound to be measured was not detected, 1 ng of a standard substance was added to the storage container, sealed, and then placed in a dry bath at room temperature (27 ° C.).

  High-purity air was used as a carrier gas, introduced from the gas inlet of the storage container, and sucked with a pump from the gas sampling port, thereby adjusting the flow rate of the carrier gas flowing through the storage container to 50 ml per minute. Carrier gas was introduced into the storage container and left for 5 minutes.

  Thereafter, a glass tube filled with Tenax (registered trademark) TA was installed as a collection tube between the gas sampling port and the pump, and 3 liters of gas released from the sample was collected.

  After collecting the carrier gas containing the diffused gas at room temperature, the sample was taken out from the storage container, and the container was sealed again. A collection tube newly filled with Tenax (registered trademark) TA in a glass tube was installed, and high-purity helium gas was introduced into the container. The high purity helium gas was introduced into the container and placed in a dry bath at 300 ° C., 3 liters of carrier gas containing the diffused gas desorbed from the storage container was discharged, and the diffused gas was collected.

  The gas component collected in the collection tube was measured with a GC / MS apparatus equipped with a heat desorption apparatus. Table 1 shows the residual ratio of each substance remaining in the storage container from the measurement result of the gas component, that is, the detected amount of each substance in the emitted gas. Here, the residual ratio is defined as a percentage obtained by subtracting the ratio of the detected amount to the added amount, assuming that the added amount of each substance added before the start of the experiment is 1.

(Comparative experiment 2)
In order to compare with the glassy carbon storage container in (Experiment 1), a quartz storage container was used, and the storage container was washed in the same manner as in (Experiment 1), and the same standard material as in (Experiment 1) was used. 1 ng was added and used, and the gas released from the sample was collected in the same procedure as in (Experiment 1) and measured with a GC / MS apparatus. The residual ratio of each substance remaining in the storage container is calculated from the measurement result of the gas component, that is, the detected amount of each substance in the emitted gas, and the result is also shown in Table 1.

  Table 1 shows the residual ratio of the components of the emitted gas, particularly the polar compound, in the storage container.

  In (Experiment 1), the residual ratio of the components of the diffused gas to the storage container is reduced to 1/2 or less than in (Comparative Experiment 1), and the storage container made of glassy carbon is particularly effective. it is obvious. By using a glassy carbon storage container, highly sensitive and highly accurate evaluation is possible. In particular, a polar compound such as 2-diethylhexyl phthalate (DOP) has a residual ratio of 2% or less, which is effective for trace analysis.

(Experiment 2)
The filter medium used for removing impurities from the air in the clean room as a sample was cut into 2 cm × 2 cm and used to measure a small amount of polar compounds. A glassy carbon storage container (30 ml) was used as the storage container, and the storage container was washed in the same manner as in (Experiment 1), and the gas emitted from the sample was collected in the same procedure as in (Experiment 1). Measured with an MS apparatus. Table 2 shows the substances detected in the emitted gas and their concentrations (μg / m ³ ) as measurement results.

(Comparative experiment 2)
In order to compare with the glassy carbon storage container of (Experiment 2), a quartz storage container was used, the storage container was washed in the same manner as in (Experiment 1), and the same filter medium as in (Experiment 2) was used as a sample. The gas emitted from the sample was collected by the same procedure as in (Experiment 1) and measured with a GC / MS apparatus. As a measurement result, the substances detected in the emitted gas and the detected amount (μg / m ³ ) are also shown in Table 2.

Table 2 shows the emitted gas components from the filter medium and the detected amount (μg / m ³ ).

  In (Experiment 2), the detected amount was larger in the glassy carbon container than in (Comparative Experiment 2), and in particular, it was prominent with a compound having polarity such as phthalate ester and low volatility.

  Moreover, when the temperature change inside a storage container was measured, the result as shown in FIG. 2 was obtained. As is clear from FIG. 2, the case of (Experiment 2) stabilizes at a predetermined temperature earlier. The storage container made of glassy carbon takes less time to adjust to the temperature suitable for the substance to be measured than the conventional container, so it is possible to reduce the denaturation of the substance to be measured. Yes, this material is suitable for trace analysis. The surface of glassy carbon is non-porous and inert, and can significantly reduce adsorption on the inner wall of the container and denaturation on the inner wall of the container, which are problematic in evaluating a small amount of emitted gas, compared to conventional storage containers. Is possible.

(Experiment 3)
Evaluation of polar compounds (emission gas) emitted from electrical appliances was performed using a container (glass-like carbon container) whose surface was coated with glassy carbon. The surface roughness of the glassy carbon used was Ra = 0.1 μm, and the surface of a 150 liter container having SiO ₂ as a support was coated with 1 mm of glassy carbon.

  The sample used was a notebook personal computer (upper (monitor part); vertical; 26 cm, horizontal; 42 cm, thickness; approximately 1 cm, lower (keyboard part); vertical; 27 cm, horizontal; 32 cm, thickness; 4 cm).

  First, the glassy carbon container was heated and washed. In a state where high purity helium gas was introduced into a glassy carbon container, it was placed in a thermostatic bath and heated at 350 ° C. for 3 hours. Thereafter, it was cooled to room temperature (27 ° C.), the background was measured by changing the carrier gas to high-purity air, and it was confirmed that the background was lower than an evaluable level.

  Next, in order to evaluate the emitted gas of the sample, the sample was placed in a container as follows. The upper part (monitor part) of the notebook personal computer is an openable type, and the monitor part is raised for normal use. The power supply was installed in a state of being turned on, sealed in a glassy carbon container, and further installed in a constant temperature bath at room temperature (27 ° C.).

  First, high-purity air was introduced from the gas inlet of the glassy carbon container and sucked with a pump so that it could be introduced into the container from the gas sampling port at a flow rate of 1.25 liter / min. After introducing high-purity air for 2 hours, another 24 hours later, a collecting tube filled with TenaxTA in a glass tube was installed between the gas sampling port and the pump, and 3 liters of gas released from the sample was collected.

  After collecting the gas released from the sample at room temperature (27 ° C.), the sample was taken out of the container, the container was sealed again, a collection tube was installed, and high purity helium gas was introduced into the container. In a state where helium gas was introduced into the container, it was placed in a constant temperature bath at 300 ° C., and 3 liters of gas was collected.

  The gas collected in the collection tube was measured by a gas chromatography / mass spectrometer with a thermal desorption device. The results are shown in Table 3.

(Comparative Experiment 3)
In order to compare with the glassy carbon container in (Experiment 3), the storage container was washed in the same manner as in (Experiment 3) using an SUS container, and the same notebook personal computer as in (Experiment 3) was used as a sample. The gas emitted from the sample was collected in the same procedure as in (Experiment 3) and measured with a GC / MS apparatus. As a measurement result, the substances detected in the emitted gas and the detected amount (μg / m ³ ) are also shown in Table 3.

  From Table 3, it was found that, particularly with respect to polar compounds such as BHT and DOP, the glassy carbon container can detect 1.3 to 1.4 in comparison with the SUS container. The surface of glassy carbon is nonporous and inert, and it can significantly reduce adsorption on the inner surface of the container and denaturation on the inner surface of the container, which are problematic in evaluating a small amount of emitted gas, compared to conventional storage containers. It is possible and effective for microanalysis.

1 is a block diagram showing a first embodiment of the present invention. The figure explaining the effect of Example 2 of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Sample, 2 ... Storage container, 3 ... Heating device, 4 ... Gas introduction port, 5 ... Gas discharge port, 6 ... Collection agent, 7 ... Collection Pipe, 8 ... Pump, 9 ... Integrated flow rate

Claims (4)

A storage container made of glassy carbon having a discharge port leading to the collection agent and storing the sample;
Discharging means for discharging the diffused gas diffused from the sample from the outlet;
And a heating means for heating the storage container after the sample is taken out.   The diffused gas discharge device according to claim 1, wherein the diffused gas from the sample is a polar compound. Diffusing volatile gas from a sample stored in a glassy carbon storage container;
Discharging the released gas in the storage container;
Collecting the exhausted exhaust gas; and
Heating the storage container from which the sample has been taken out, discharging the residual gas remaining on the inner surface of the storage container, and collecting the discharged residual gas;
A method for collecting emitted gas, comprising:   The method for collecting a diffused gas according to claim 3, wherein the diffused gas is a polar compound.

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