JP3792682B2 - Sample container discharge device - Google Patents

Description

  The present invention relates to a sample container discharging apparatus that discharges a sample container accommodated in a thermal analyzer from the thermal analyzer after the analysis is completed.

  In order to analyze the composition and microstructure of a polymer sample, a gas component generated by heating the polymer sample is introduced into an analyzer such as a gas chromatograph device or a mass spectrometer and analyzed. Yes. For the analysis, for example, a thermal analyzer 2 having a configuration shown in FIG.

  The thermal analysis apparatus 2 includes a heating furnace 5 including a quartz pyrolysis tube 3 provided in the vertical direction and a heater 4 disposed on the outer periphery of the quartz pyrolysis tube 3, and a lower end of the quartz pyrolysis tube 3. The unit is connected to an analyzer 6 such as a gas chromatograph or a mass spectrometer. A carrier gas inlet 9 for introducing a carrier gas into the quartz pyrolysis tube 3 is provided above the quartz pyrolysis tube 3, and a sample sampler 31 is fitted into the upper opening of the quartz pyrolysis tube 3. It has become. The sample sampler 31 includes gripping means 33 for gripping a sample container 32 in which a polymer sample is accommodated, and is fitted to the upper opening to close the upper opening.

  When the polymer sample is heated by the thermal analyzer 2, first, as shown in FIG. 11A, the sample sampler 32 is held in a state where the sample container 32 containing the polymer sample is held by the holding means 33. 31 is fitted into the upper opening of the quartz pyrolysis tube 3. The sample container 32 includes a container main body 34 that is a bottomed cylindrical hollow body, and a handle portion 35 that is welded to a side wall portion of the container main body 34, and an end portion of the handle portion 35 is held by the holding means 33. Yes.

  Next, the gripping means 33 is operated to release the gripping of the handle portion 35, and as shown in FIG. 11 (b), the sample container 32 is freely dropped into the quartz pyrolysis tube 3 to thereby produce a quartz pyrolysis tube. A polymer sample is introduced into 3. At this time, since the heating furnace 5 is heated to a temperature of about 500 to 800 ° C., for example, the polymer sample is instantaneously pyrolyzed to generate a gas component. The gaseous component is guided to the analyzer 6 by the carrier gas introduced from the carrier gas inlet 9 and analyzed.

  When the analysis is completed, the sample sampler 31 is removed and the sample container 32 is recovered from the heating furnace 5 as shown in FIG. Conventionally, the operation of recovering the sample container 32 is performed by inserting a sample container recovery device 37 having a flange 36 at the tip from the upper opening of the quartz pyrolysis tube 3 and inserting the flange 36 into the handle 35 of the sample container 32. It is carried out by hooking it up on a stop rod 38 provided on the top and pulling it up.

  However, since the heater 4 is disposed on the outer peripheral portion of the quartz pyrolysis tube 3 as described above, the collar portion 36 of the sample container recovery tool 37 is fixed to the handle portion 35 of the sample container 32. The operation of hooking on 38 cannot be visually observed and must be carried out by groping. For this reason, there exists a problem that the said operation requires a high degree of skill.

  In order to solve the above problem, the present applicant includes an elastic portion 40 at the tip of a handle 39 having a length that can reach the sample container 32 introduced into the quartz pyrolysis tube 3, as shown in FIG. A sample container recovery device 41 is proposed, and the sample container recovery device 41 has already been patented (see Patent Document 1). According to the sample container recovery device 41, when inserted into the quartz pyrolysis tube 3 from the upper opening of the quartz pyrolysis tube 3, the elastic portion 40 is crimped to the sample container 32 as shown in phantom lines in FIG. The sample container 32 can be held only by doing this. Therefore, the operation of recovering the sample container 32 from the quartz pyrolysis tube 3 can be easily performed after the analysis is completed.

However, even if the sample container collection device 41 is used, the operation of introducing the sample container 32 into the quartz pyrolysis tube 3 and manually collecting it after the end of the analysis is performed, and improvement in operating efficiency is desired.
Japanese Patent No. 3321382 Japanese Patent No. 2742492

  The present invention has been made in view of such circumstances, and it is possible to discharge an analyzed sample container from a heating furnace of a thermal analysis device without manual operation, thereby improving the operation efficiency of the thermal analysis device. An object of the present invention is to provide a sample container discharging apparatus capable of performing

  In order to achieve such an object, the present invention provides a sample container for discharging a sample container after the analysis of the sample from a thermal analyzer that analyzes the sample by heating the sample contained in the sample container. The thermal analysis apparatus includes a tubular body provided in the vertical direction, a sample container inlet provided at an upper end portion of the tubular body, and the tubular body via the sample container inlet. A heating furnace for heating the sample introduced into the tubular body by a heating means provided on the outer peripheral side of the tubular body to vaporize the sample, and a gas generated by vaporization of the sample connected to the lower end of the tubular body An analysis means for performing the analysis of, and the discharge device is provided between the lower end of the heating furnace and the analysis means, and after the analysis of the sample is completed, a high-pressure gas is introduced into the tubular body, The sample container is moved above the tubular body against gravity, and the sample container Characterized in that it comprises a high-pressure gas introducing means for discharging from the sample container inlet.

  In the sample container discharging apparatus of the present invention, when the sample is heated in the heating furnace and the analysis of the sample is completed, a high-pressure gas is introduced into the tubular body by the high-pressure gas introduction unit. The gas passes through the heating furnace and forms an air flow toward the sample inlet, but since the gas is at a high pressure, the sample container accommodated in the heating furnace resists gravity by the air flow. Then, it is moved above the tubular body. Then, the sample container is discharged to the outside from the sample introduction port.

  Therefore, according to the sample container discharge apparatus of the present invention, the analyzed sample container can be discharged from the heating furnace of the thermal analysis apparatus without manual operation, and the operating efficiency of the thermal analysis apparatus can be improved. it can.

  By the way, when the sample is made of a polymer resin or the like, it contains a low-molecular component such as a plasticizer in addition to the polymer component serving as the base of the resin. It is desirable to clarify not only the composition of the high molecular component but also the composition of the low molecular component. However, when the sample is heated at a temperature at which the polymer component is thermally decomposed by the thermal decomposition apparatus, the low molecular component is further degraded by thermal decomposition of the molecules constituting the component itself or by causing a chemical reaction. Therefore, it is difficult to separate the low molecular components from each other.

  Therefore, first, the sample is heated to a temperature at which the low molecular component vaporizes in the heating furnace, and the vaporized component is analyzed, and then the sample is put on standby at a position where it is not heated. There is a thermal analyzer in which after heating to a temperature at which it is instantly pyrolyzed, the sample is again introduced into the heating furnace and pyrolyzed to analyze the generated gas component (see, for example, Patent Document 2). .

For use in such a thermal analysis apparatus, the sample container discharging apparatus according to the present invention further comprises an opening / closing means for opening and closing the tubular body at a position between the heating furnace and the sample container inlet. And the tubular body between the heating furnace and the opening / closing means is provided to be openable and closable, and the high-pressure gas is introduced into the tubular body from the high-pressure gas introduction means with the opening / closing means closing the tubular body. The high-pressure gas discharge means that is opened when the high-pressure gas is discharged, and the tubular body between the heating furnace and the high-pressure gas discharge means is provided so as to freely advance and retreat into the tubular body. The high pressure gas is introduced into the tubular body from the high pressure gas introducing means in a state in which the tubular body is closed and the high pressure gas discharging means is opened, and the sample container is resisted by gravity and above the tubular body. When moving to the tubular body, the high-pressure gas causes the tube to enter the tubular body. Ru and a sample container detention means for placing a Moved sample reservoir above the body.

Prior Sharing, ABS sensing device, wherein the sample in the heating furnace is heated, after the analysis of low-molecular components is performed vaporized, while closing the tubular member by the switching means, opening the high-pressure gas discharge means In this state, the high pressure gas is introduced into the tubular body by the high pressure gas introducing means. In this case, since the tubular body is closed at a position between the heating furnace and the sample introduction port, the high-pressure gas passes through the heating furnace, and the heating furnace and the opening / closing means An air flow toward the high-pressure gas discharge means provided in the tubular body in between is formed.

  At this time, since the gas is at a high pressure, the sample container accommodated in the heating furnace is moved above the tubular body against the gravity by the airflow. Blocked by means. Therefore, the sample container is not discharged to the outside from the sample introduction port, but remains between the heating furnace and the high-pressure gas discharge means.

  Then, the sample container can be placed on the tubular body by the advancement of the sample container placing means into the tubular body.

  Next, in the discharge apparatus having the above-described configuration, after the high-pressure gas introduction by the high-pressure gas introduction unit is stopped and the high-pressure gas discharge unit is closed, the polymer component contained in the sample is pyrolyzed in the heating furnace. Is heated to a temperature. When the sample container indwelling means is retracted from the tubular body, the sample container is again introduced into the heating furnace, and the polymer component is thermally decomposed.

  Next, when the analysis of the gas component generated by thermal decomposition of the polymer component is completed, the opening / closing means is opened, and the high-pressure gas is introduced into the tubular body by the high-pressure gas introduction means. As a result, the high-pressure gas passes through the heating furnace to form an air flow toward the sample introduction port, and the sample container accommodated in the heating furnace resists gravity due to the air flow. The sample is moved upward and further discharged from the sample inlet.

  The sample container discharging apparatus of the present invention further includes a sample container holding means for holding the sample container above the sample container inlet, and the sample container held by the sample container holding means is connected to the sample container inlet. It is preferable to provide a sample container introducing means for introducing into the thermal analysis device by allowing it to freely fall into the tubular body via the.

  In the discharging apparatus having the above configuration, the sample container held by the sample container holding means is dropped freely from the sample container introduction port into the tubular body by the sample container introduction means and introduced into the thermal analysis apparatus. . Therefore, all operations from introducing the sample container into the thermal analyzer and discharging it after completion of the analysis can be automated, and the operating efficiency of the thermal analyzer can be significantly improved.

  Next, embodiments of the present invention will be described in more detail with reference to the accompanying drawings. FIG. 1 is an explanatory cross-sectional view showing the configuration of the sample container discharge device of the present embodiment, FIG. 2 is an explanatory cross-sectional view showing in detail the main part of the discharge device shown in FIG. 1, and FIGS. It is action | operation explanatory drawing of the discharge device shown in FIG.

  As shown in FIG. 1, a sample container discharge device 1 of this embodiment is used for a thermal analysis device 2, and the thermal analysis device 2 includes a quartz pyrolysis tube 3 provided in a vertical shape, and a quartz thermal decomposition device. A heating furnace 5 including a heater 4 disposed around the decomposition tube 3 and an analyzer 6 such as a gas chromatograph apparatus and a mass spectrometer connected to the lower end of the heating furnace 5 are provided. A tubular sample introduction portion 7 is connected above the quartz pyrolysis tube 3, and the upper end opening of the sample introduction portion 7 serves as a sample introduction port 8.

  A carrier gas introduction port 9 for introducing a carrier gas such as helium gas or air into the quartz pyrolysis tube 3 is provided at the lower part of the sample introduction unit 7, and a carrier introduced from the carrier gas introduction port 9 is provided at the upper part. A carrier gas discharge port 10 for discharging a part of the gas is provided. A sample container indwelling device 11 is provided between the carrier gas introduction port 9 and the carrier gas discharge port 10 so as to be able to advance and retreat with respect to the sample introduction unit 7.

  In contrast to the thermal analyzer 2 having the above-described configuration, the sample container discharge device 1 includes a high-pressure gas inlet 12 that communicates with the quartz pyrolysis tube 3 between the heating furnace 5 and the analyzer 6, and a carrier gas discharge port 10. A switch 13 that opens and closes the sample introduction unit 7, a high-pressure gas discharge port 14 that communicates with the carrier gas discharge port 10, and a sample. The sample container introducing device 15 is provided above the introduction port 8. As the high-pressure gas, for example, helium gas can be used, but high-pressure air may be used.

  The high pressure gas inlet 12 is connected to a high pressure gas source 17 via an on-off valve 16. The high-pressure gas discharge port 14 is provided with an on-off valve 18.

  Further, as shown in FIG. 2, the sample container introducing device 15 includes a disk-shaped sample container holder 21 provided with a plurality of through holes 20 for accommodating a cup-shaped sample container 19 and rotatably provided, and a sample. A disc-shaped bottom plate 23 provided with a sample container dropping port 22 attached to the lower part of the container holder 21 and communicating with the sample introduction port 8, and a sample container dropping port provided to be movable forward and backward with respect to the bottom plate 23. And a shutter 24 that opens and closes 22.

  In the sample container introducing device 15, the bottom plate 23 is fixed at a position where the sample container dropping port 22 communicates with the sample introducing port 8, and only the sample container holder 21 is driven by a stepping motor or the like so as to rotate by a predetermined angle. It has become. At this time, although the sample container 19 is accommodated in the through hole 20, the bottom of the through hole 20 is normally in contact with the bottom plate 23, so that the sample container 19 does not fall. Then, when the sample container dropping port 22 is opened by the shutter 24 when the predetermined sample container 19 comes on the sample container dropping port 22, the through-hole 20 passes through the sample container dropping port 22 and the sample introduction port 8. The sample container 19 falls into the sample introduction port 8 due to its own weight.

  Next, referring to FIG. 3 to FIG. 10, the sample container discharging apparatus 1 of the present embodiment when the low molecular component in the polymer sample is first vaporized by the thermal analyzer 2 and then the polymer component is thermally decomposed. Will be described. 3 to 10 schematically show the configuration of the sample container introducing device 15.

  First, as shown in FIG. 3, in the initial state, both the on-off valve 16 of the high-pressure gas inlet 12 and the on-off valve 18 of the high-pressure gas outlet 14 are closed, and the switch 13 closes the sample introduction unit 7, The shutter 24 closes the sample container dropping port 22. On the other hand, a carrier gas such as helium is always introduced from the carrier gas introduction port 9, a part of which flows into the sample introduction unit 7 and is discharged from the carrier gas discharge port 10, and the remaining part passes through the quartz pyrolysis tube 3. To the analyzer 6.

  Next, as shown in FIG. 4, when the switch 13 is retracted to open the sample introduction unit 7 and the sample container dropping port 22 is opened by the shutter 24, the sample container dropping port 22 is positioned at this time. The sample container 19 falls freely into the sample introduction part 7 by its own weight. And the sample container 19 is detained on the sample container detainer 11.

  When the sample container 19 is introduced into the sample introduction unit 7 in this way, air enters the sample introduction unit 7 along with the sample container 19. If air is present when the polymer sample stored in the sample container 19 is heated, an undesired reaction may occur, for example, the vaporized component may be oxidized by oxygen in the air.

  Then, as shown in FIG. 5, the switch 13 is advanced to close the sample introduction part 7, while the sample container dropping port 22 is closed by the shutter 24. In this way, the air that has entered the sample container 19 is discharged out of the apparatus by the carrier gas that is always introduced from the carrier gas inlet 9 as described above.

  Next, when the air is discharged as described above, the sample container indwelling device 11 is moved backward while the sample introduction unit 7 is closed by the switch 13 as shown in FIG. If it does in this way, the sample container 19 indwelled on the sample container indwelling device 11 will fall freely in the heating furnace 5 with dead weight. And the low molecular component in the polymer sample accommodated in the sample container 19 is vaporized by heating and heating in the heating furnace 5 at a temperature in the range of 50 to 300 ° C., for example. The gas component generated by the vaporization is introduced into the analyzer 6 by the carrier gas introduced from the carrier gas inlet 9 and analyzed.

  Next, when the analysis of the gas component generated by the heating and heating is completed, as shown in FIG. 7, the on-off valve 16 of the high-pressure gas inlet 12 and the on-off valve 18 of the high-pressure gas outlet 14 are opened. Thus, a high-pressure gas such as high-pressure helium gas is introduced into the heating furnace 5 from the high-pressure gas source 12 through the high-pressure gas inlet 12. At this time, the sample introduction part 7 is closed by the switch 13, but the high-pressure gas discharge port 14 is opened, so that the high-pressure gas forms an air flow from the heating furnace 5 toward the high-pressure gas discharge port 14. As a result, the sample container 19 is moved from the heating furnace 5 into the sample introduction unit 7 against gravity by the airflow.

  Then, next, as shown in FIG. 8, the sample container 19 is moved into the sample introduction part 7 by the air flow by moving the sample container indweller 11 to the sample introduction part 7. Place in place. Then, the on-off valve 16 of the high-pressure gas inlet 12 and the on-off valve 18 of the high-pressure gas outlet 14 are closed, and the introduction of the high-pressure gas is stopped.

  Next, while the sample container 19 is indwelling on the sample container indwelling device 11, the temperature of the heating furnace 5 is raised to a range of 500 to 800 ° C., for example. Then, as shown in FIG. 9, the sample container detainer 11 is retracted while the sample introduction unit 7 is closed by the switch 13, and the sample container 19 that has been detained on the sample container detainer 11 is heated. Free fall into the furnace 5. In this way, the polymer component in the polymer sample contained in the sample container 19 is instantly pyrolyzed, and the gas component generated by the pyrolysis is absorbed by the carrier gas introduced from the carrier gas inlet 9. It is introduced into the analysis device 6 and analyzed.

  Next, when the analysis of the gas component generated by the thermal decomposition is completed, the sample introduction part 7 is opened by the on-off valve 13 and the sample container dropping port 22 is opened by the shutter 23 as shown in FIG. Then, with the on-off valve 18 of the high-pressure gas discharge port 14 closed, the on-off valve 16 of the high-pressure gas inlet 12 is opened. In this way, the high-pressure gas introduced into the heating furnace 5 from the high-pressure gas source 12 through the high-pressure gas inlet 12 forms an airflow from the heating furnace 5 through the sample introduction part 7 toward the sample container dropping port 22. . As a result, the sample container 19 is moved upward from the heating furnace 5 against the gravity by the airflow, and further discharged out of the apparatus through the sample container dropping port 22. The sample container 19 is collected in a collection container 25 or the like provided outside the sample container introduction device 15.

  In the sample container discharge device 1, when the sample container 19 is discharged from the heating furnace 5, the on-off valve 16 of the high-pressure gas inlet 12 and the on-off valve 18 of the high-pressure gas outlet 14 are closed to introduce high-pressure gas. To stop. Then, the switch 13 closes the sample introduction unit 7, the shutter 24 closes the sample container dropping port 22, and the sample container indwelling device 11 advances into the sample introduction unit 7, whereby the initial state shown in FIG. Return to.

  Next, in the sample container discharge device 1, the sample container holder 21 is rotated to move the next sample container 19 onto the sample container dropping port 22. Then, the operations of FIGS. 3 to 10 are repeated.

  In the present embodiment, the case where the low molecular component in the polymer sample is first vaporized and then the high molecular component is thermally decomposed is described. However, the sample container discharge device 1 of the present embodiment vaporizes the low molecular component. It can also be used when the polymer sample is immediately pyrolyzed without any problems. In this case, the steps of FIGS. 6 to 8 described above may be omitted, and the steps of FIGS. 9 and 10 may be performed immediately after the step of FIG.

Explanatory sectional drawing which shows one structural example of the discharge apparatus of the sample container of this invention. Explanatory sectional drawing which shows the principal part of the discharge device shown in FIG. 1 in detail. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Operation | movement explanatory drawing of the discharge device shown in FIG. Explanatory sectional drawing which shows the example of 1 structure of a thermal analyzer. The perspective view which shows the conventional sample container collection | recovery tool.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Sample container discharge device, 2 ... Thermal analysis device, 3, 7 ... Tubular body, 4 ... Heating means, 5 ... Heating furnace, 6 ... Analysis means, 8 ... Sample introduction port, 11 ... Sample container placement means, 12 DESCRIPTION OF SYMBOLS ... High pressure gas introduction means, 13 ... Opening / closing means, 14 ... High pressure gas discharge means, 15 ... Sample container introduction means, 19 ... Sample container, 21 ... Sample container holding means.

Claims (2)

A sample container discharge device that discharges the sample container after the analysis of the sample from a thermal analyzer that analyzes the sample by heating the sample contained in the sample container,
The thermal analysis apparatus includes a tubular body provided in a vertical direction, a sample container introduction port provided at an upper end portion of the tubular body, and the sample introduced into the tubular body via the sample container introduction port. A heating furnace that is heated by a heating means provided on the outer peripheral side of the tubular body to vaporize the sample, and an analysis means that is connected to the lower end of the tubular body and analyzes the gas generated by vaporization of the sample; With
The discharge device is provided between the lower end portion of the heating furnace and the analysis means, and after the analysis of the sample is completed, a high-pressure gas is introduced into the tubular body, so that the sample container is resisted by gravity and the tubular High-pressure gas introduction means for moving the sample container upward from the body and discharging the sample container from the sample container inlet ;
Opening and closing means for freely opening and closing the tubular body at a position between the heating furnace and the sample container inlet;
When the high-pressure gas is introduced into the tubular body from the high-pressure gas introduction means with the tubular body between the heating furnace and the open-close means being freely opened and closed, and the open-close means closes the tubular body A high-pressure gas discharge means that is opened to discharge the high-pressure gas;
In the tubular body between the heating furnace and the high-pressure gas discharge means, the tubular body is provided so as to be able to advance and retreat, and the opening and closing means closes the tubular body and opens the high-pressure gas discharge means, When high pressure gas is introduced into the tubular body from the high pressure gas introducing means, and the sample container is moved above the tubular body against gravity, the sample container advances into the tubular body, A sample container discharge device comprising: a sample container indwelling means for indwelling the sample container moved above the tubular body . A sample container holding means for holding the sample container above the sample container inlet, and the sample container held by the sample container holder is freely dropped into the tubular body through the sample container inlet. The sample container discharging apparatus according to claim 1, further comprising a sample container introducing unit that introduces the thermal analyzer.

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