JP7142374B2 - Gas phase component analyzer and gas phase component analysis method - Google Patents

Description

The present invention relates to a gas phase component analysis device and a gas phase component analysis method.

Gas chromatography is conventionally known as a method for analyzing gas phase components. As a gas phase component analyzer (gas chromatograph) used for gas chromatography, for example, a heating means for heating a sample to generate a gas phase component mixture, and the gas generated by the heating means connected to the heating means. A separation column that separates a phase component mixture into individual components, a constant temperature bath (oven) that houses the separation column, and a detector that is connected to the separation column and detects the components separated by the separation column. things are known.

The heating means thermally decomposes or volatilizes the sample, or heats the sample to thermally desorb components contained in the sample to generate the gas phase component mixture. A mass spectrometry detector (MS), a flame ionization detector (FID), an electron capture detector (ECD), or the like is used as the detector.

When analyzing a dilute sample having a sample concentration of less than 0.01% by mass in the gas phase component analyzer, 90% by mass or more of the gas phase component mixture produced as described above is introduced into the separation column. analysis. However, in this case, the separation column is deteriorated by unreacted methylating agent such as TMAH (tetramethylanmonium hydride) used when the gas phase component mixture contains carboxylic acid, or the separation column is deteriorated by silylation such as HMDS (hexamethyldisilazane). There is a problem that the sensitivity of a flame ionization detector (FID) used as the detector changes depending on the agent. In addition, in the gas phase component analysis device, when the gas phase component mixture is injected into the separation column in an amount 10 to 50 times the usual amount for the purpose of high-sensitivity detection, when a mass spectrometry detector (MS) is used as a detector has a problem that a large amount of solvent flows into the mass spectrometry detector (MS), which makes it impossible to maintain a high vacuum, resulting in malfunction.

In order to solve the above-mentioned problems, the heating means is provided with a split vent so that part of the gas phase component mixture is selectively introduced into the separation column while the rest is discharged to the outside. A gas-phase component analyzer is known (see Patent Document 1, for example).

The gas phase component analyzer described in Patent Document 1, when analyzing a sample having a sample concentration of 0.01 mass% or more, 90 to 99% of the gas phase component mixture generated as described above is externally discharged from the split vent. 1 to 10% of the gas phase component mixture is introduced into the separation column for analysis. As a result, according to the gas-phase component analyzer described in Patent Document 1, unnecessary components such as the methylating agent, the silylating agent, and the solvent can be discharged to the outside, and only the component to be analyzed can be introduced into the separation column. can.

JP 2018-66618 A

However, the gas-phase component analyzer described in Patent Document 1 has the problem that the detection sensitivity decreases when the amount of the gas-phase component mixture introduced into the separation column decreases.

The present invention is a gas phase component analyzer and a gas phase component analyzer that can eliminate such inconveniences, prevent deterioration of the separation column and detector due to unnecessary non-analyte components, and can obtain excellent detection sensitivity. An object is to provide a component analysis method.

In order to achieve such an object, the gas phase component analyzer of the present invention
Equipped with a pyrolysis furnace, a heater arranged around the pyrolysis furnace, and a GC inlet into which the tip of the pyrolysis furnace is inserted, and housed in a sample cup put into the pyrolysis furnace a heating device for heating a solid sample as a sample with the heater to generate a gas phase component mixture;
a first column, one end of which is inserted into the GC injection port and faces the tip of the pyrolysis furnace, into which the gas phase component mixture produced by the heating device is introduced;
a second column, which is a separation column, connected to the first column via connecting means;
a constant temperature bath containing the first column, the second column, and the connection means;
A gas phase component analyzer comprising a detection means for detecting a gas phase component that has passed through the second column,
It is characterized by comprising suction means connected to the connection means.

Further, the gas phase component analysis method of the present invention is a gas phase component analysis method using the gas phase component analysis device,
When the solid sample as the sample is heated by the heater in the heating device to generate the gas phase component mixture, the sample contained in the sample cup is transferred to the pyrolysis furnace after the suction means is operated. , and the suction means is operated for a predetermined period of time from the time the sample is charged , and the non-analyte component is discharged outside through the suction means, while the temperature of the first column is reduced to the non-analytical a step of selectively trapping the analyte component in the first column at a temperature higher than the boiling point of the target component and lower than the boiling point of the analyte component;
A step of stopping the suction means after the predetermined time, raising the temperature of the constant temperature bath to a temperature equal to or higher than the boiling point of the component to be analyzed, and introducing the component to be analyzed into the second column. Characterized by

In the gas phase component analysis apparatus and gas phase component analysis method of the present invention, first, the sample is heated by the heating means to thermally decompose or volatilize the sample, or thermally desorb the gas phase components from the sample. , to produce the gas phase component mixture. At this time, when the sample is charged or injected into the heating means after the suction means is operated, and the suction means is operated for a predetermined time after the sample is charged or injected, the gas phase component mixture is sucked. and the entire gas phase mixture is introduced into the first column. The gas phase component mixture contains a high boiling point, low volatility analyte component and a low boiling point, high volatility non-analyte component such as a solvent, wherein the first column has a boiling point of the non-analyte component Since the temperature is higher than the boiling point of the analyte component, the non-analyte component is sucked further toward the suction means without being captured by the first column, while the analyte component is selected. effectively trapped in the first column.

Here, said first column is connected to said second column via said connection means, and said suction means is also connected to said connection means. However, since the second column acts as a flow path resistance, the non-analyte components are not introduced into the second column, but are sucked into the suction means and released to the outside through the suction means. be done.

After the non-analyte component is released to the outside, the suction means is stopped after the predetermined time, and the temperature of the constant temperature bath is raised to a temperature equal to or higher than the boiling point of the analyte component. In this way, the analyte trapped in the first column is vaporized and moves towards the connecting means. At this time, since the suction means is stopped and the direction of connecting the connection means to the suction means is closed, the vaporized analyte component is introduced into the second column. . Since the second column is a separation column, the analyte components introduced into the second column are separated into individual gas phase components, and the individual gas phase components that have passed through the second column are separated into the Detected by the detection means.

As described above, in the gas phase component analysis apparatus and the gas phase component analysis method of the present invention, the entire amount of the gas phase component mixture generated by the heating means is introduced into the first column, but non-aqueous substances such as solvents are introduced into the first column. While the analyte component is released to the outside, the analyte component is trapped in the first column, concentrated, and then introduced into the second column. Therefore, according to the gas-phase component analyzer and the gas-phase component analysis method of the present invention, it is possible to prevent deterioration of the separation column and detector due to unnecessary non-analyte components such as solvents, and to achieve excellent detection sensitivity. Obtainable.

The gas phase component analyzer of the present invention includes selective introduction means ( backflush device, etc.) may be provided at the GC inlet .

Further, in the gas phase component analysis method of the present invention, the predetermined time as the time for further operating the suction means from the time when the sample is put into the pyrolysis furnace is a time in the range of 1 second to 3 minutes. Preferably, the non-analyte components can be reliably released to the outside. If the predetermined time is less than 1 second from the time the sample is put into the pyrolysis furnace, the non-analyte component cannot be sufficiently released to the outside, and the time exceeds 3 minutes from the time the sample is put or injected. However, no further effect is obtained.

Further, in the gas phase component analysis method of the present invention, when the temperature of the first column is higher than the boiling point of the non-analyte component and lower than the boiling point of the analyte component, the first column is cooled to ensure that the temperature of the first column is below the boiling point of the analyte.

An explanatory cross-sectional view showing one configuration example of the gas phase component analyzer of the present invention. FIG. 4 is an explanatory cross-sectional view showing another configuration example of the gas phase component analyzer of the present invention. The figure which shows one analysis example by the gas phase component analysis apparatus of this invention, and a gas phase component analysis method. FIG. 4 is a diagram showing another example of analysis by the gas phase component analysis device and gas phase component analysis method of the present invention; FIG. 5 is a diagram showing still another example of analysis by the gas phase component analysis apparatus and gas phase component analysis method of the present invention;

Embodiments of the present invention will now be described in more detail with reference to the accompanying drawings.

As shown in FIG. 1, the gas phase component analyzer 1 of this embodiment is a gas chromatograph, and includes a heating device 2, a constant temperature bath 3 connected to the heating device 2, and a detection device connected to the constant temperature bath 3. 4.

The heating device 2 includes a pyrolysis furnace 21 made of a chemically inert hollow cylindrical quartz tube, a heater 22 provided around the pyrolysis furnace 21, and a GC into which the tip of the pyrolysis furnace 21 is inserted. and an inlet 23 . The heater 22 heats the pyrolysis furnace 21 under predetermined conditions by means of a temperature control device (not shown). The pyrolysis furnace 21 is connected to the top of the GC inlet 23 with a heated pipe or the like, or is detachably attached. Further, the pyrolysis furnace 21 may be composed of a stainless steel tube made inert by forming a quartz thin film on the inner surface thereof instead of the quartz tube.

The GC injection port 23 is provided with a heater (not shown) which, like the heater 22, heats the GC injection port 23 under predetermined conditions by a temperature control device (not shown). If the pyrolysis furnace 21 is not connected or attached to the top of the GC inlet 23, a septum (not shown) is attached to the upper end.

The heating device 2 includes a sample introduction section 24 connected above the pyrolysis furnace 21, and a carrier gas conduit 25 as carrier gas introduction means for introducing a carrier gas into the pyrolysis furnace 21 is connected to the sample introduction section 24. It is The other end of carrier gas conduit 25 is connected to carrier gas source 27 via flow controller 26 . Also, the carrier gas conduit 25 is connected to the GC inlet 23 when the pyrolysis furnace 21 is not connected or mounted above the GC inlet 23 .

As a result, the carrier gas supplied from the carrier gas source 27 is adjusted to a predetermined flow rate by the flow controller 26 and introduced into the pyrolysis furnace 21 or the GC inlet 23 .

The constant temperature bath 3 has a pre-column 31 as a first column, a main separation column 32 as a second column which is a separation column, and a three-way pipe as connecting means for connecting the pre-column 31 and the main separation column 32. (T-tube) 33 is accommodated. One end of the pre-column 31 is inserted into the GC injection port 23 and faces the tip of the pyrolysis furnace 21 , while the other end is connected to the main separation column 32 via a three-way pipe 33 . The main separation column 32 has one end connected to the pre-column 31 via a three-way tube 33 and the other end connected to a detection means 41 such as a quadrupole mass spectrometry detector housed in the detection device 4 . ing.

The three-way pipe 33 connects the pre-column 31 and the main separation column 32 in a straight line, and is connected to the exhaust conduit 34 in a direction orthogonal to the connection direction between the pre-column 31 and the main separation column 32. is connected to a suction pump 5 such as a vacuum pump provided outside the constant temperature bath 3 .

The pre-column 31 has, for example, an inner diameter of 0.25 mm, a length of 1 m, and a fixed layer of thickness 0.25 μm made of a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95 on the inner surface. or a capillary column with an inner diameter of about 0.1 to 0.5 mm and a length of 0.5 to 19 m, the inner surface of which is coated with various polymers, or the inner surface of which is chemically inactivated without coating the polymer. A capillary tube can be used. The main separation column 32 has, for example, an inner diameter of 0.25 mm, a length of 30 m, and a thickness of 0.2 mm made of a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95. A stainless steel capillary column with a 25 μm fixed bed can be used.

The pre-column 31 is detachable from the GC injection port 23 and the three-way tube 33, and the pre-column 31 can be selected according to the object to be analyzed.

As the detection means 41, a mass spectrometry detector (MS) such as the quadrupole mass spectrometry detector, a flame ionization detector (FID), an electron capture detector (ECD), or the like can be used.

Next, the gas phase component analysis method of this embodiment using the gas phase component analysis device 1 shown in FIG. 1 will be described.

In the gas phase component analysis method of the present embodiment, first, a carrier gas such as helium or nitrogen is supplied from the carrier gas source 27 through the flow control device 26 to the pyrolysis furnace 21 at a flow rate of 5 to 150 ml / min. The heater 22 heats the pyrolysis furnace 21 to a predetermined temperature. Next, after operating the suction pump 5, the solid sample or liquid sample contained in the sample cup 6 is put into the heating furnace 21 to thermally decompose the solid sample, volatilize the liquid sample, or A gas phase mixture is produced by thermally desorbing the gas phase components from the sample.

Further, when the pyrolysis furnace 21 is not connected or attached to the upper part of the GC inlet 23, the liquid sample or gas sample is injected from the septum into the GC inlet 23 using a microsyringe (not shown) and heated. A liquid sample or the gas sample can be stripped to produce a gas phase component mixture.

Next, the suction pump 5 is operated for a predetermined period of time, for example, for a period of 1 second to 3 minutes from when the sample is introduced or injected, and the entire amount of the gas phase component mixture is introduced into the pre-column 31. At this time, the pre-column 31 is controlled to a predetermined temperature by the constant temperature bath 3, or cooled by a coolant such as liquid nitrogen, liquid carbon dioxide, ice, etc., to a temperature higher than the boiling point of the non-analyte component contained in the gas phase component mixture. It is defined as a temperature lower than the boiling point of the component to be analyzed. As a result, highly volatile non-analyte components such as solvents are not captured by the pre-column 31 and are further sucked in the direction of the suction pump 5, while the components to be analyzed are selectively captured by the pre-column 31 and concentrated. be done.

Here, the pre-column 31 is connected to the main separation column 32 via a three-way tube (T-tube) 33, and the suction pump 5 is also connected to the three-way tube 33 via an exhaust conduit 34. Since the separation column 32 acts as a flow path resistance, the non-analyte components are not substantially introduced into the main separation column 32, but are sucked by the suction means pump 5 via the exhaust conduit 34 and discharged to the outside. be. When the main separation column 32 is connected to a mass spectrometry detector (MS), the inside of the mass spectrometry detector is evacuated, so that a small amount of the non-analyte component is introduced into the main separation column 32. However, since the introduced non-analyte component is in a very small amount, it does not cause deterioration of the main separation column 32 or malfunction of the mass spectrometry detector.

Next, when the suction pump 5 is stopped after the predetermined time and the temperature of the constant temperature bath 3 is raised to a temperature equal to or higher than the boiling point of the component to be analyzed, the component to be analyzed trapped in the pre-column 31 is vaporized and Move in the direction of the directional tube 33 . At this time, the suction pump 5 acts as a valve in the exhaust conduit 34, and since the suction pump 5 is stopped and the valve is closed, the vaporized component to be analyzed can be removed by controlling the flow rate of the carrier gas. It is introduced into the main separation column 32 , separated into individual gas phase components, and detected by the detection means 41 .

As described above, according to the gas phase component analysis method of the present embodiment using the gas phase component analyzer 1, non-analyte components such as solvents are released to the outside, while the target components are trapped in the pre-column 31. , is introduced into the main separation column 32 after being concentrated, so that deterioration of the main separation column 32 and the detection means 41 due to the non-analyte components can be prevented, and excellent detection sensitivity can be obtained.

As shown in FIG. 2, the gas phase component analyzer 1 may be provided with a split vent 35 as a selective introduction means for selectively introducing the gas phase component mixture into the pre-column 31 at the GC inlet 23. . The split vent 35 introduces a part of the gas phase component mixture introduced from the pyrolysis furnace 21 or produced at the GC inlet 23 into the pre-column 31 and discharges the remainder to the outside through an exhaust pipe 36 .

According to the gas-phase component analyzer 1 shown in FIG. 90 to 99% of the gas phase component mixture produced at the inlet 23 is released to the outside, and 1 to 10% of the gas phase component mixture is introduced from the precolumn 31 into the main separation column 32 for analysis. Further, when the gas phase component analyzer 1 having the split vent 35 is used for the gas phase component analysis method of the present embodiment, first, the split vent 35 is closed for 5 seconds to 5 minutes, the suction pump 5 is operated, and then While supplying a carrier gas such as helium or nitrogen from a carrier gas source 27 to the pyrolysis furnace 21 at a flow rate of 5 to 150 ml/min through a flow control device 26, the sample is introduced into the heating furnace 21 or the GC inlet 23. Alternatively, it is injected, thermally decomposed, volatilized or thermally desorbed to produce a gas phase component mixture. By operating the suction pump 5, the split vent 35 does not substantially operate, and after the suction pump 5 is stopped, the split vent 35 operates normally, and the carrier gas whose flow rate is controlled as described above is supplied. Since it is introduced into the pre-column 31, it can operate in the same manner as the gas phase component analyzer 1 shown in FIG.

Next, an example is shown.

[Example 1]
In this example, first, a hexane solution containing a hydrocarbon having 9 to 22 carbon atoms and an ester thereof at a concentration of 500 ppm each was prepared and used as a sample.

Next, using the gas phase component analyzer 1 shown in FIG. 2, 1 μL of the sample was injected into the GC injection port 23 with a microsyringe, and the sample was volatilized to generate a gas phase component mixture.

In this embodiment, in the gas phase component analyzer 1, the pre-column 31 has an inner diameter of 0.25 mm, a length of 1 m, and a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95 on the inner surface. A stainless steel capillary column with a fixed layer having a thickness of 0.25 μm is used. A stainless steel capillary column (manufactured by Frontier Labs, trade name: UA5-30M-0.25F) provided with a 0.25 μm-thick fixed layer made of a copolymer having a molar ratio) was used. As the detection means 41, a quadrupole mass spectrometry detector (scan range: m/z 10-400) was used.

In the analysis, a carrier gas was supplied from the carrier gas source 26 to the GC injection port 23 at a flow rate of 1.0 mL/min through the flow controller 25, and the split ratio of the split vent 35 was 1/10 (introduced gas phase components 1/10 of this is introduced into the pre-column 31), the temperature of the GC injection port 23 is 350 ° C., and the temperature of the constant temperature bath 3 is held at 40 ° C. for 2 minutes, and then heated to 300 ° C. at a temperature increase rate of 20 ° C./min. I did it on condition. The analysis results when the suction pump 5 was not operated at all are shown in the upper part of FIG. The analysis results are shown in the lower part of FIG.

From FIG. 3, when the suction pump 5 was not operated at all, a solvent peak appeared in the retention time range of 1 to 5 minutes, and the absolute intensity was 1×10 ⁷ . When the pump 5 is operated, the suction pump 5 is operated for 10 seconds after sample injection, and then stopped, the solvent peak is not observed at all, and the absolute intensity is 1×10 ⁸ , which is 10 times greater. Above, each hydrocarbon is also clearly separated, and it is clear that excellent detection sensitivity can be obtained.

[Example 2]
In this example, first, a dichloromethane solution containing 0.5 μg/μL of polystyrene with an average molecular weight of 300,000 and 0.05 μg/μL of methyl stearate as an internal standard was prepared as a sample.

Next, using the gas phase component analyzer 1 shown in FIG. 2, 5 μL of the sample is collected in the sample cup 6, the solvent is volatilized at room temperature (25° C.), and then placed in the heating furnace 21 heated to 600° C. and the sample was pyrolyzed to produce a gas phase mixture.

In this embodiment, in the gas phase component analyzer 1, the pre-column 31 has an inner diameter of 0.25 mm, a length of 2 m, and a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95 on the inner surface. A stainless steel capillary column (manufactured by Frontier Laboratories, Inc., trade name: Ultra ALLOY 50) with a fixed layer of 1.0 μm in thickness is used as the main separation column 32. A stainless steel capillary column with a 0.5 μm-thick fixing layer made of a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95 (manufactured by Frontier Labs, trade name: Ultra ALLOY+ -5) was used. A quadrupole mass spectrometry detector (scan range: m/z 29-350) was used as the detection means 41 .

In the analysis, the carrier gas (helium) was supplied from the carrier gas source 26 to the heating furnace 21 at a flow rate of 1.0 mL/min through the flow controller 25, the split ratio of the split vent 35 was 1/16, and the GC inlet 23 The temperature was 300° C., and the temperature of the constant temperature bath 3 was held at 40° C. for 2 minutes, then heated to 280° C. at a rate of 20° C./min, and held at 280° C. for 6 minutes. The analysis results obtained when the suction pump 5 was not operated at all are shown in the upper part of FIG. The analysis results are shown in the lower part of FIG.

In addition, when the suction pump 5 is operated, after a part of the pre-column 31 is immersed in liquid nitrogen in advance, the suction pump 5 is operated and then stopped, the pre-column 31 is pulled up from the liquid nitrogen, and the temperature of the constant temperature bath 3 is changed. was heated under the above conditions.

From FIG. 4, when the suction pump 5 is operated before the sample is added, and the suction pump 5 is operated for 10 seconds after the sample is added, and then stopped, the comparison is made when the suction pump 5 is not operated at all. The absolute intensity increased tenfold, from 1×10 ⁶ to 1×10 ⁷ , and the peak area increased 12.4 times for methyl stearate and 17.6 times for styrene trimer, demonstrating excellent detection. It is clear that sensitivity can be obtained.

[Example 3]
In this example, first, a sample containing 300 μg of polyethylene, 2 μg of nylon 6,6, and 80 μg of polypropylene was prepared.

Next, using the gas phase component analysis apparatus 1 shown in FIG. 2, the sample is placed in the sample cup 6 and put into the heating furnace 21 heated to 600° C. to thermally decompose the sample into gas phase components. A mixture was formed.

In this embodiment, in the gas phase component analyzer 1, the pre-column 31 has an inner diameter of 0.25 mm, a length of 1 m, and a copolymer of methylphenylpolysiloxane and dimethylpolysiloxane at a molar ratio of 5:95 on the inner surface. A first stainless steel capillary column with a 0.5 μm thick fixed layer consisting of, or an inner diameter of 0.25 mm, a length of 2 m, and a 50:50 (molar ratio) of methylphenylpolysiloxane and dimethylpolysiloxane on the inner surface The same gas phase component analyzer 1 as in Example 2 was used except that a second stainless steel capillary column having a fixed layer of 1.0 μm in thickness made of a copolymer of was used.

The analysis was performed under exactly the same conditions as in Example 2, the suction pump 5 was operated before the sample was added, and the suction pump 5 was operated for 10 seconds after the sample was added, and then stopped.

The analysis results when the first stainless steel capillary column was used as the pre-column 31 are shown in the upper part of FIG. 5, and the analysis results when the second stainless steel capillary column was used as the pre-column 31 are shown in the lower part of FIG. The analysis result of this example is an selective ion chromatogram (EIC) when only the mass ion m/z 84 is selected in the pyrogram with a retention time range of 5.2 to 6.8 minutes.

In the thermal decomposition of the sample, polyethylene produced C8' having 8 carbon atoms and one double bond and saturated hydrocarbon C8 having 8 carbon atoms, cyclopentanone was produced from nylon 6,6, and polypropylene A trimer of propylene (propylene trimer) is produced from the Here, when the first stainless steel capillary column shown in the upper part of FIG. 5 is used, the peak at the retention time of 5.9 minutes is a mixture of two components, C8' and cyclopentanone. In polymer qualitative analysis, improved separation is sought for polymer qualitative analysis of polyethylene and nylon 6,6 using C8' and cyclopentanone.

Therefore, various studies were made on the pre-column 31, and when the second stainless steel capillary column with an increased polar group concentration was used, it was found that C8' and cyclopentanone could be completely separated as shown in the lower part of FIG. it is obvious.

In the gas-phase component analysis method using a separation column, there are many cases where a plurality of compounds are overlapped and detected without being separated even when a high-resolution main separation column 32 having a length of 30 m or more is used. In such cases, it becomes necessary to change the polarity of the liquid phase applied to the main separation column 32 in order to improve the separation of the multiple components. However, for that purpose, it is required to prepare a new main separation column 32 and to conduct the analytical examination again, which requires a great deal of labor and associated costs.

On the other hand, in the gas phase component analysis method of the present embodiment, the effect of improving separation can be obtained simply by changing the pre-column 31 according to the object to be analyzed. It is possible to greatly reduce the labor and the cost associated with it.

REFERENCE SIGNS LIST 1 gas phase component analyzer 2 heating means 3 constant temperature bath 4 detection means 5 suction means 31 first column 32 second column 33 connecting means 35 selective means of introduction.

Claims (5)

Equipped with a pyrolysis furnace, a heater arranged around the pyrolysis furnace, and a GC inlet into which the tip of the pyrolysis furnace is inserted, and housed in a sample cup put into the pyrolysis furnace a heating device for heating a solid sample as a sample with the heater to generate a gas phase component mixture;
a first column, one end of which is inserted into the GC injection port and faces the tip of the pyrolysis furnace, into which the gas phase component mixture produced by the heating device is introduced;
a second column, which is a separation column, connected to the first column via connecting means;
a constant temperature bath containing the first column, the second column, and the connection means;
A gas phase component analyzer comprising a detection means for detecting a gas phase component that has passed through the second column,
A gas-phase component analyzer, comprising suction means connected to the connection means. In the gas phase component analyzer according to claim 1,
The GC injection port is provided with selective introduction means for selectively introducing a part of the gas phase component mixture generated by the heating device into the first column and discharging the remainder to the outside. Gas phase component analyzer. Equipped with a pyrolysis furnace, a heater arranged around the pyrolysis furnace, and a GC inlet into which the tip of the pyrolysis furnace is inserted, and housed in a sample cup put into the pyrolysis furnace a heating device for heating the sample with the heater to generate a gas phase component mixture;
a first column, one end of which is inserted into the GC injection port and faces the tip of the pyrolysis furnace, into which the gas phase component mixture produced by the heating device is introduced;
a second column, which is a separation column, connected to the first column via connecting means;
a constant temperature bath containing the first column, the second column, and the connection means;
A gas phase component analyzer comprising a detection means for detecting a gas phase component that has passed through the second column,
A gas phase component analysis method using a gas phase component analysis device provided with suction means connected to the connection means,
When the solid sample as the sample is heated by the heater in the heating device to generate the gas phase component mixture, the sample contained in the sample cup is transferred to the pyrolysis furnace after the suction means is operated. , and the suction means is operated for a predetermined period of time from the time the sample is charged , and the non-analyte component is discharged outside through the suction means, while the temperature of the first column is reduced to the non-analytical a step of selectively trapping the analyte component in the first column at a temperature higher than the boiling point of the target component and lower than the boiling point of the analyte component;
A step of stopping the suction means after the predetermined time, raising the temperature of the constant temperature bath to a temperature equal to or higher than the boiling point of the component to be analyzed, and introducing the component to be analyzed into the second column. Gas phase component analysis method characterized. In the gas phase component analysis method according to claim 3,
The gas phase component analysis method, wherein the predetermined time is in the range of 1 second to 3 minutes after the sample is put into the pyrolysis furnace . In the gas phase component analysis method according to claim 3 or claim 4,
Gas phase component analysis, wherein the first column is cooled with a refrigerant when the temperature of the first column is set to a temperature higher than the boiling point of the non-analyte component and lower than the boiling point of the analyte component. Method.

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