JP2007232646A - Discharge device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a discharge device separating excellently a sample gas from a sample body. <P>SOLUTION: In an aging device 10, a collecting tube 14 is stored in a heating furnace 74 and heated, and thereby the sample gas is eliminated from a scavenger 12 in the collecting tube 14 and the collecting tube 14 is aged. In this case, in a humidifier 28, cleaning gas penetrates through a liquid holding part 56 for holding a humidifying agent, and thereby the humidifying agent is changed into fine particles by the cleaning gas and discharged into a space layer 60, while particles of the humidifying agent passing the space layer 60 penetrates through a liquid stopping part 62, and thereby discharged to the front side of the liquid stopping part 62 in the colorless transparent state. Hereby, the cleaning gas is humidified properly and supplied into the collecting tube 14, so that the sample gas is eliminated excellently from the scavenger 12. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a discharge device that desorbs a sample gas from a sample body in a sample container and discharges the sample gas to the outside of the sample container.

  As the discharge device, the gas from which the adsorbed component (sample gas) in the gas component adsorption tube is desorbed by heating the gas component adsorption tube with the oven while allowing the cleaning gas to pass through the gas component adsorption tube installed in the oven. There is a component adsorption tube cleaning device (see, for example, Patent Document 1).

  However, in this gas component adsorption tube cleaning apparatus, the gas component adsorption tube is installed in the oven by inserting and holding the gas component adsorption tube in a state where the gas component adsorption tube is aligned in a bottomed hole provided in the oven. For this reason, it is necessary to manually align the gas component adsorption tube with the bottomed hole, and the operation of installing the gas component adsorption tube in the oven is complicated. For this reason, gas component adsorption tubes having different diameters and types but different types cannot be installed in the oven.

  The cleaning gas that passes through the gas component adsorption tube is dried. For this reason, the adsorption component in the gas component adsorption tube cannot be desorbed satisfactorily.

  Furthermore, when the passage resistance of the cleaning gas in the plurality of gas component adsorption pipes is different from each other, the gas component adsorption pipe having a higher passage resistance of the cleaning gas cannot pass through the cleaning gas and desorbs the adsorption component well. I can't.

In addition, when the temperature in the oven is controlled to the set temperature based on the detection of the temperature in the oven by the temperature sensor, since the heater capacity of the oven is generally large, the temperature in the oven becomes lower than the set temperature. When the inside of the oven is temporarily heated, the temperature inside the oven becomes higher than the set temperature, causing overheating (overshoot) of the gas component adsorption tube or becoming unstable.
Japanese Patent Laid-Open No. 10-185891

  In consideration of the above facts, the present invention provides a discharge device that can favorably desorb a sample gas from a sample body, a discharge device that can easily dispose a sample container on a heating means, and a small heating capacity of a heat generating portion of the heating means. Discharge device capable of supplying supply gas satisfactorily not only to a sample container having a low supply gas passage resistance but also to a sample vessel having a high supply gas passage resistance, and a plurality of types of sample containers from a sample body The object is to obtain a discharge device that can desorb the sample gas.

  The discharge device according to claim 1 is connected to a sample container in which a sample body from which a sample gas is desorbed by heating is connected, and supplies a supply gas into the sample container; Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container; and provided in the supply means for holding the liquid and transmitting the supply gas Liquid holding part, a space part arranged on the sample container side of the liquid holding part, and a liquid which is arranged on the sample container side of the space part and reaches from the liquid holding part through the space part is a particle And a humidifying means having a discharge portion that is formed and discharged to the sample container side together with the supply gas.

  The discharge device according to claim 2 is the discharge device according to claim 1, wherein the humidifying means stores the liquid retaining portion, and seals the storage container provided with the injection port and the injection port. And a hermetically sealed portion that is capable of injecting a liquid into the liquid retaining portion.

  The discharge device according to claim 3 is the discharge device according to claim 1 or 2, wherein the supply means supplies gas into the sample container even after liquid is no longer held in the liquid holding section. It is characterized by supplying.

  The discharge device according to claim 4 is connected to a sample container in which a sample body from which a sample gas is desorbed by heating is connected, and supplies a supply gas into the sample container; A heating means for detaching the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container; and a placement of the sample container on the heating means supporting the sample container Guiding means for guiding.

  The discharge device according to claim 5 is the discharge device according to claim 4, wherein the supply means can supply supply gas into the plurality of sample containers simultaneously, and the heating means includes a plurality of The sample container can be heated at the same time.

  The discharge device according to claim 6 is connected to a sample container in which a sample body from which a sample gas is desorbed by heating is connected, a supply means for supplying a supply gas into the sample container, and heat generation And a heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container.

  The discharge device according to claim 7 is the discharge device according to claim 6, further comprising an additional heat generating portion that is provided in the heating means and generates heat when the heating temperature of the heating means is increased. It is said.

  The discharge device according to claim 8 has a plurality of branch portions connected to each of a plurality of sample containers provided therein with a sample body from which the sample gas is desorbed by being heated, and the sample container A supply means for supplying a supply gas therein, a plurality of resistance means for providing resistance to the supply gas passing through the branch portions, respectively, and heating the sample container. Heating means for desorbing the sample gas from the sample body and discharging the sample gas from the sample container.

  The discharge device according to claim 9 is provided with connection means connected to a sample container in which a sample body from which a sample gas is desorbed by heating is provided, and supplies a supply gas into the sample container Supply means for heating, and heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container, and connecting a plurality of types of the sample containers It is characterized in that it can be exchanged and connected to the means.

  The discharge device according to claim 10 is provided with connection means connected to a sample container in which a sample body from which a sample gas is desorbed by heating is provided, and supplies a supply gas into the sample container Supply means, and heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container. It is characterized in that a plurality of different types of connection means can be exchanged and installed in the supply means.

  The discharge device according to claim 11 is connected to a sample container in which a sample body from which a sample gas is desorbed by heating is connected, and supplies a supply gas into the sample container; A heating container for holding the sample container is attached, and heating means for detaching the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container is capable of being accommodated A plurality of types of heating containers having different types of sample containers can be exchanged and attached to the heating means.

  In the discharge device according to claim 1, the supply means supplies the supply gas into the sample container, and the heating means heats the sample container, whereby the sample gas is desorbed from the sample body in the sample container, and the sample is removed. Discharged from the container.

  Here, the supply means is provided with a humidifying means having a liquid holding part, a space part and a discharge part, and the liquid holding part holds the liquid and allows the supply gas to pass therethrough, and the space part is a sample of the liquid holding part. The liquid which is arranged on the container side and reaches the discharge part from the liquid holding part through the space part is made into particles by the discharge part and discharged to the sample container side together with the supply gas. For this reason, the supply gas can be appropriately humidified, and the sample gas can be favorably desorbed from the sample body.

  In the discharge device according to the second aspect, in the humidifying means, the storage container stores the liquid retaining portion, and the storage container is provided with an inlet. A sealing part is hermetically provided at the inlet, and the sealing part can inject liquid into the liquid retaining part. For this reason, a liquid can be easily inject | poured into a liquid holding part.

  In the discharge device according to the third aspect, the supply means supplies the supply gas into the sample container even after the liquid is no longer held in the liquid holding section. For this reason, after supplying the humidified supply gas into the sample container, the dry supply gas can be supplied.

  In the discharge device according to claim 4, the supply means supplies the supply gas into the sample container, and the heating means heats the sample container, whereby the sample gas is desorbed from the sample body in the sample container, and the sample is removed. Discharged from the container.

  Here, the guide means supports the sample container and guides the arrangement of the sample container on the heating means. For this reason, a sample container can be easily arrange | positioned to a heating means.

  In the discharge device according to the fifth aspect, the supply means can simultaneously supply the supply gas into the plurality of sample containers, and the heating means can simultaneously heat the plurality of sample containers. Therefore, the sample gas can be desorbed from the sample body at the same time in a plurality of sample containers.

  In the discharge device according to claim 6, the supply means supplies the supply gas into the sample container, and the heating means generates heat in the heat generating portion to heat the sample container, whereby the sample gas is removed from the sample body in the sample container. Is desorbed and discharged from the sample container.

  Here, the heating means has a plurality of heat generating portions. For this reason, the heat generation capacity of the heat generating part can be reduced, and the heating temperature of the heating means can be stabilized by increasing the heat storage capacity of the heating means.

  In the discharge device according to the seventh aspect, the additional heat generating portion provided in the heating unit generates heat when the heating temperature of the heating unit is increased. For this reason, the heating temperature of a heating means can be raised rapidly.

  In the discharge device according to claim 8, the supply unit supplies the supply gas into the plurality of sample containers through the plurality of branch portions, and the heating unit heats the sample container, whereby the sample body in the sample container is provided. The sample gas is desorbed from and discharged from the sample container.

  Here, the resistance means provided in each of the plurality of branch portions imparts resistance to the supply gas passing through the branch portions. For this reason, even when the flow resistances of the supply gases in a plurality of sample containers are different from each other, the supply gas is satisfactorily supplied not only to a sample container having a low supply gas passage resistance but also to a sample container having a high supply gas passage resistance Can do.

  In the discharge device according to claim 9, the sample container is connected to the connecting means provided in the supply means, the supply means supplies the supply gas into the sample container, and the heating means heats the sample container, The sample gas is desorbed from the sample body in the sample container and discharged from the sample container.

  Here, a plurality of types of sample containers can be exchanged and connected to the connecting means. Therefore, the sample gas can be desorbed from the sample body with respect to a plurality of types of sample containers.

  In the discharge device according to claim 10, the sample container is connected to the connection means provided in the supply means, the supply means supplies the supply gas into the sample container, and the heating means heats the sample container, The sample gas is desorbed from the sample body in the sample container and discharged from the sample container.

  Here, a plurality of types of connection means having different types of connectable sample containers can be exchanged and installed in the supply means. Therefore, the sample gas can be desorbed from the sample body with respect to a plurality of types of sample containers.

  In the discharge device according to claim 11, the supply means supplies the supply gas into the sample container, and the heating means heats the sample container accommodated in the heating container, so that the sample gas is removed from the sample body in the sample container. Is desorbed and discharged from the sample container.

  Here, a plurality of types of heating containers having different types of sample containers that can be accommodated can be exchanged and attached to the heating means. For this reason, a different kind of sample container can be accommodated in a heating container by replacing | exchanging the heating container attached to a heating means. Thereby, the sample gas can be desorbed from the sample body with respect to a plurality of types of sample containers.

  FIG. 1 shows a side view of an aging device 10 as a discharge device according to an embodiment of the present invention viewed from the left side, and FIG. 2 is a plan view of the aging device 10 viewed from above. Is shown. In the drawing, the front of the aging device 10 is indicated by an arrow FR, the right side of the aging device 10 is indicated by an arrow RH, and the upper side of the aging device 10 is indicated by an arrow UP.

  For example, in order to reduce VOC (Volatile Organic Compounds) in the passenger compartment, it is necessary to grasp the volatilization amount (generated amount) of VOC for each material used in the passenger compartment.

  As a method for analyzing a volatilized sample gas such as VOC (a target component such as hydrocarbons), a glass container (made of stainless steel) having a sample body filled with, for example, a resin collector 12 as a sample body is used. Some may use a circular collection tube 14. That is, by holding (collecting) the sample gas in the collection agent 12 through the sample gas in the collection tube 14, heating the collection tube 14 in a state connected to a so-called gas chromatograph as an analyzer, The sample gas (holding component) is desorbed (vaporized) from the collecting agent 12 and analyzed by a gas chromatograph. The method of concentrating the sample gas by holding it in the collection agent 12 in the collection tube 14 in this way is a collection method that is frequently used in the air collection or the like. It can be concentrated to several milliliters, so that the sensitivity of the analysis can be enhanced, and the sample gas is excellent in storability and transportability.

  In addition, the collection tube 14 after the analysis process is heated to, for example, approximately 300 ° C., and the sample gas (residual component) remaining from the collection agent 12 is desorbed (removed), thereby aging (washing). ) And reused for analytical processing.

  The aging device 10 according to the present embodiment is for aging the collection tube 14. The aging device 10 includes a rectangular plate-like base 16, and a plurality of rectangular parallelepiped legs 18 are fixed to the lower surface of the base 16. Thus, the aging device 10 is placed on the placement surface in a state where the base 16 is leveled by placing the plurality of legs 18 on a horizontal placement surface (not shown).

  A first rail 20 is provided at the center of the upper surface of the base 16 in the left-right direction except for the front end portion, and the first rail 20 is disposed along the front-rear direction. Further, a second rail 22 is provided at the right end of the upper surface of the base 16 except for the front end portion, and the second rail 22 is disposed along the front-rear direction.

  On the first rail 20, a fixture 24 as a moving means is disposed at the rear part. A rectangular plate-like slide portion 24A is provided on the lower portion of the fixture 24. The slide portion 24A is supported by the first rail 20 so as to be slidable (movable). It is guided by the rail 20 and is slidable in the front-rear direction. A plate-like fixing portion 24B is provided on the upper portion of the fixing tool 24, and the fixing portion 24B is erected vertically from the slide portion 24A. A plurality (six in this embodiment) of circular fixing holes 26 are formed in the fixing portion 24B, and the fixing portion 24B has a humidifying portion that constitutes a branching portion of the supply means in each fixing hole 26. A cylindrical humidifier 28 as a means is fixed in a fitted state.

  On the second rail 22, a front-reverse L-shaped guide 30 as a guide means is disposed at the front portion. The lower end of the guide 30 is slidably supported by the second rail 22, whereby the guide 30 is guided by the second rail 22 to be slidable in the front-rear direction, and the upper portion 30 </ b> A of the guide 30 is It is arranged horizontally in front of the fixture 24.

  The humidifier 28 is connected to one end of a resistance tube 34 constituting a branch portion of the supply means and a resistance means via a branch pipe 32 constituting a branch portion of the supply means from the rear surface. While being held by the slide portion 24A of the fixture 24, the diameter is made smaller than the diameter of the supply pipe 36 described below. As shown in detail in FIG. 4, the other end of each resistance tube 34 is connected to a supply tube 36 that constitutes a supply means, whereby a plurality of resistance tubes 34 are branched from the supply tube 36. ing.

  The supply pipe 36 is provided with a gas cleaning section 38. Further, the supply pipe 36 is provided with a pressure control section (flow rate control section) on the side opposite to the resistance pipe 34 (upstream side) from the gas cleaning section 38. The pressure gauge 40 and the pressure adjustment valve 42 which are comprised are provided in order toward the anti-gas cleaning part 38 side. Thereby, the cleaning gas (inert gas such as air, nitrogen or helium) as the supply gas is controlled by the pressure adjustment valve 42 and confirmed by the pressure gauge 40 and cleaned by the gas cleaning unit 38. While being supplied from the supply pipe 36 to the humidifiers 28 through the resistance pipes 34 and the branch pipes 32, they are supplied at a constant pressure and a low flow rate. Further, when the cleaning gas passes through the resistance tube 34, resistance is given to the cleaning gas by the resistance tube 34 (the passage of the cleaning gas is hindered).

  The outer periphery of the humidifier 28 is a cylindrical container-like storage container 44, and the cleaning gas is supplied into the storage container 44 from the branch pipe 32. An injection port 46 having a circular shape when viewed from above is formed through the upper portion and the rear portion of the peripheral wall of the storage container 44, and the injection port 46 is sealed by a rubber partition wall 48 as a sealing portion. The inlet 46 may be configured to be sealed with a screw-type or cap-type sealing lid. In this case, the inlet 46 can be opened by removing the sealing lid from the inlet 46.

  As shown in detail in FIG. 6, an orifice 50 that constitutes resistance means is provided at the rear of the storage container 44, and the orifice 50 is fitted in the storage container 44. The orifice 50 is provided with a layered filter 52 on the rear side, and the cleaning gas supplied into the storage container 44 passes through the filter 52 to be cleaned. The orifice 50 is provided with a film-like liquid stop film 54 on the front side, and the liquid stop film 54 permeates the cleaning gas and prevents permeation of the following humidifier due to the backflow. In addition, the orifice 50 (the filter 52 and the liquid stop film 54) provides resistance to the permeating cleaning gas (inhibiting permeation of the cleaning gas). Note that the filter 52 and the liquid stop film 54 can be used together.

  A column-shaped liquid retaining part 56 is provided in the intermediate portion in the front-rear direction in the container 44, and the liquid retaining part 56 is fitted in a cylindrical recovery part 58 (drain liquid recovery part). . The collection unit 58 is fitted to the inner peripheral surface of the storage container 44. The liquid retaining part 56 and the collecting part 58 are made of a liquid retaining material such as a filter medium such as a Teflon (registered trademark) membrane, glass fiber, chemical fiber, ceramic, etc., and the liquid retaining part 56 and the collecting part 58 (liquid retaining part). If the material is highly lyophobic, it must be lyophilic. Although a space is formed between the liquid retaining portion 56 and the liquid stop film 54 of the orifice 50, this space may not be formed.

  The water injection port 46 is disposed on the upper side of the liquid retaining part 56, and the liquid retaining part 56 has a thin tubular (injection needle-like) injection tube (injection needle shape) provided in a syringe-like injector (not shown). In the state where the illustration is omitted) penetrates the partition wall 48 of the injection port 46, a humidifying agent (water or a substance having a high polarity such as organic compounds such as various alcohols) is injected (supplied) through the injection tube. ) As a result, the moisturizer is held in the liquid retaining portion 56, and the moisturizer particles are held and arranged in the entire cross section by capillary action. Further, when the penetration of the injection tube into the partition wall 48 is released, the partition wall 48 seals the injection port 46. Furthermore, even if the moisturizing agent retained in the liquid retaining unit 56 penetrates into the collecting unit 58, it is prevented from leaking to the rear side from the orifice 50 by the liquid stop film 54 of the orifice 50, and also due to capillary action. It is collected in the liquid retaining unit 56.

  The cleaning gas that has passed through the orifice 50 passes through the liquid retaining unit 56, and the retained humidifier is made fine particles by the cleaning gas and discharged to the front side.

  In the container 44, a space layer 60 is formed as a space portion in the collecting portion 58 on the front side of the liquid retaining portion 56, and the humidifier for fine particles discharged from the liquid retaining portion 56 is formed in the space layer 60. Pass through. When the particles of the humidifying agent passing through the space layer 60 are large and fall to the collecting unit 58, they are held by the collecting unit 58 and collected by the liquid retaining unit 56 by capillary action.

  In the storage container 44, a liquid stop part 62 as a discharge part is provided on the front side of the space layer 60. The liquid stop part 62 is fitted in the storage container 44 and contacts the recovery part 58. Has been. The liquid stopping part 62 is composed of a porous liquid stopping material formed in the shape of a gas permeable material (filter), and the moisturizing agent particles that have passed through the space layer 60 pass through the liquid stopping part 62. It becomes a uniform optimum particle shape, and is discharged to the front side of the liquid stopping part 62 in a colorless and transparent state (a state dissolved in the cleaning gas). Furthermore, since the space layer 60 is disposed on the rear side of the liquid stopping portion 62, it is prevented that a particle film is formed on the entire rear surface of the liquid stopping portion 62 due to the particles of the humidifying agent that has passed through the space layer 60. Yes. Further, when the particles of the humidifying agent that have passed through the space layer 60 are large and cannot pass through the liquid stopping part 62, they are dropped and held in the collecting part 58, and are collected in the liquid retaining part 56 by capillary action.

  An adapter 64 (attachment) as a connecting means (connector) constituting a branching portion of the supply means is detachably attached to the front surface of the storage container 44. As shown in FIG. 8, the adapter 64 has a so-called syringe needle having a so-called caulking type adapter 64A having a so-called ferrule, an abacus ball (engagement cylinder) and an O-ring, and a narrow tubular (injection needle-shaped) communication tube 66. A type adapter 64B exists, and a caulking type adapter 64A or a syringe needle type adapter 64B can be exchangeably attached to the front surface of the container 44.

  The adapter 64 is connected to the rear end of the collection tube 14 that has finished the analysis process. The rear end of the collection tube 14 serves as a supply port 68 and the front end of the collection tube 14 serves as a discharge port. 70. As a result, the cleaning gas humidified by the humidifier in the humidifier 28 is supplied from the supply port 68 to the collection tube 14 via the adapter 64, and the cleaning gas passes through the collection tube 14 and is discharged. It is discharged from the outlet 70.

  When the collection tube 14 is a so-called straight tube collection tube 14 (hereinafter referred to as “straight tube collection tube 14 </ b> A”) in which the supply port 68 and the discharge port 70 are opened, a caulking is formed on the front surface of the storage container 44. By attaching the type adapter 64A and connecting the straight pipe collection pipe 14A to the caulking type adapter 64A, the inside of the straight pipe collection pipe 14A and the inside of the storage container 44 are communicated with each other through the caulking type adapter 64A. The Further, a plurality of types of straight pipe collecting pipes 14A having different outer diameters can be connected to the caulking type adapter 64A.

  On the other hand, when the collection tube 14 is a so-called rubber seal type collection tube 14 (hereinafter referred to as “rubber seal collection tube 14B”) in which the supply port 68 is sealed by the rubber 72 and the discharge port 70 is opened, The syringe needle type adapter 64B is attached to the front surface of the storage container 44, and the rubber seal collecting tube 14B is connected to the syringe needle type adapter 64B in a state where the communication pipe 66 of the syringe needle type adapter 64B is penetrated by the rubber 72. Thus, the inside of the rubber seal collecting tube 14B and the inside of the storage container 44 are communicated with each other through the inside of the syringe needle type adapter 64B (including the inside of the communicating tube 66). Further, a plurality of types of rubber seal collecting tubes 14B having different outer diameters can be connected to the syringe needle type adapter 64B.

  As shown in FIGS. 1 and 2, the front portion of the collection tube 14 connected to the adapter 64 is placed and supported on the upper portion 30 </ b> A of the guide 30, whereby the collection tube 14 is In the front part, it is restrained from hanging down and is arranged horizontally.

  A rectangular parallelepiped heating furnace 74 as a heating means is fixed on the base 16 at the front end. A plurality of tubular heating pipes 76 as heating containers are detachably attached to the heating furnace 74, and the plurality of heating pipes 76 penetrate the heating furnace 74 in the front-rear direction and are each a collection pipe. 14 in the front-rear direction. The heating tube 76 is made of stainless steel when strength is required, whereas the heating tube 76 is made of glass when the sample gas held in the collecting agent 12 in the opposing collecting tube 14 is a corrosive gas. It is made of quartz.

  A plurality of types of heating tubes 76 as shown in FIGS. 9A to 9D can be exchanged and attached to the heating furnace 74, and the inner surface of the heating tube 76 is a heater surface 76A. All types of heating tubes 76 have a predetermined outer diameter (for example, 10 mm), and the heating tube 76 is in the same state as the heating furnace 74 no matter which type of heating tube 76 is attached to the heating furnace 74 ( The heating tube 76 and the heating furnace 74 can be attached in the same state). Different types of heating tubes 76 have different inner diameters (for example, changed within a range of 6 mm or more and 9 mm or less), and the heating tube 76 attached to the heating furnace 74 has a larger outer diameter than the opposing collection tube 14. The inner diameter is larger by a predetermined length (for example, 1 mm or more and 4 mm or less).

  As shown in FIG. 10, a thermal fuse 78 is provided in the heating furnace 74, and a power supply 80 is electrically connected to the thermal fuse 78. The temperature fuse 78 is electrically connected to a temperature setting unit 82 and a temperature control unit 84 (temperature control device) that are electrically connected to each other. The temperature control unit 84 is a so-called liquid-filled type or side temperature. It has a simple configuration such as a resistance type. The temperature control unit 84 is provided with a power switch 86 that enables the heating furnace 74 to be turned on and off, and a temperature display unit 88.

  In the heating furnace 74, a plurality of main heaters 90 as heat generating units are provided, and the main heaters 90 are electrically connected to the temperature control unit 84 while the heater capacity (heat generating capacity) is reduced. . A predetermined number of sub-heaters 92 as additional heat generating units are provided in the heating furnace 74, and the sub-heaters 92 have a heater capacity larger than that of the main heater 90 and are electrically connected to the temperature control unit 84. ing. A temperature sensor 94 is provided in the heating furnace 74. The temperature sensor 94 detects the temperature in the heating furnace 74 and is electrically connected to the temperature control unit 84. The display 88 can display the temperature in the heating furnace 74.

  A heat storage material 96 as a heat storage means is provided in the heating furnace 74, and the heat storage material 96 is disposed in substantially the entire space in the heating furnace 74 to increase the heat storage capacity in the heating furnace 74. Yes.

  Next, the operation of the present embodiment will be described.

  In the aging device 10 configured as described above, when the power switch 86 of the heating furnace 74 is turned ON, power is supplied from the power source 80 to at least one of the main heater 90 and the sub heater 92 via the temperature fuse 78 and the temperature control unit 84. By being supplied and at least one of the main heater 90 and the sub heater 92 generates heat, the inside of the heating furnace 74 (including the heating pipe 76 and the heat storage material 96) is heated.

  The temperature control unit 84 controls the power supply to the main heater 90 and the sub-heater 92 based on the temperature in the heating furnace 74 detected by the temperature sensor 94, thereby setting the temperature in the heating furnace 74 to the temperature setting unit 82. To the set temperature set at (up to about 300 ° C.). Further, when the temperature in the heating furnace 74 becomes abnormally high, the power supply from the power source 80 to the temperature control unit 84 is interrupted by the thermal fuse 78.

  Further, in a state where the temperature in the heating furnace 74 is maintained at the set temperature, as shown in FIG. 3, the fixture 24 is slid forward while being guided by the first rail 20, and the humidifier 28, the adapter 64 and the trap 64 are captured. The collection tube 14 is accommodated in the heating tube 76 of the heating furnace 74 by sliding the collection tube 14 forward. At this time, the guide 30 is slid forward while being guided by the second rail 22, and the collection tube 14 is maintained on the upper portion 30 </ b> A of the guide 30, so that the collection tube 14 is guided by the guide 30. And is accommodated in the heating tube 76. Thus, the collection tube 14 is accommodated in the heating tube 76 and the collection tube 14 is heated, so that the sample gas remaining in the collection agent 12 in the collection tube 14 is removed from the collection agent 12. Separated and discharged from the outlet 70 of the collection tube 14, and the collection tube 14 is aged.

  Further, when the collection tube 14 is accommodated in the heating tube 76 of the heating furnace 74 and heated, the cleaning gas is controlled by the pressure adjusting valve 42 and the pressure gauge 40 confirms the supply pressure, While being cleaned by the gas cleaning unit 38, the gas is supplied from the supply pipe 36 through the resistance pipe 34 and the branch pipe 32 into the housing container 44 of the humidifier 28. Thereby, the cleaning gas passes through the container 44 and is humidified by the humidifying agent held in the liquid retaining unit 56, and is supplied from the supply port 68 to the collection tube 14 via the adapter 64. The cleaning gas passes through the collection tube 14 and is discharged from the discharge port 70. For this reason, the sample gas (including high boiling point components and components strongly held by the collection agent 12) is desorbed from the collection agent 12 in the collection tube 14 and the collection tube 14 is excellent. Aged.

  Here, the cleaning gas can be simultaneously supplied from the supply pipe 36 to the plurality of collection pipes 14 via the plurality of resistance pipes 34, the plurality of branch pipes 32, the plurality of humidifiers 28, and the plurality of adapters 64. . Further, the heating furnace 74 can accommodate the plurality of collecting tubes 14 in the plurality of heating tubes 76 so that the plurality of collecting tubes 14 can be heated simultaneously. For this reason, in addition to the collection tube 14 in which the sample gas is held in the collection agent 12 in one analysis process, the sample tube is not held in the collection tube 14 for creating a so-called calibration curve and the collection agent 12. Even when a plurality of collection tubes 14 such as blank collection tubes 14 are used, the plurality of collection tubes 14 can be aged simultaneously.

  Furthermore, resistance is given to the cleaning gas which the resistance tube 34 provided between the supply pipe 36 and each humidifier 28 passes, and it resists the cleaning gas which the orifice 50 provided in each humidifier 28 permeate | transmits. Is granted. Therefore, even when the inner diameter (shape) and the packing density / filling amount of the collecting agent 12 are different from each other in the plurality of collecting tubes 14 and the passage resistance of the cleaning gas is different, the collection resistance of the cleaning gas is low. An approximately same amount of the cleaning gas can be simultaneously supplied not only to the tube 14 but also to the collecting tube 14 having a high passage resistance of the cleaning gas, and the aging effect on the plurality of collecting tubes 14 (background to the collecting agent 12) (Residual rate) can be made equal.

  Moreover, even if the collection pipe 14 is not connected to some of the adapters 64, the part of the adapters 64 is similar to the branch path from the supply pipe 36 to the other adapter 64 to which the collection pipe 14 is connected. The orifice 50 and the resistance pipe 34 also provide resistance to the cleaning gas in the branch path from the supply pipe 36 to the pipe. For this reason, the cleaning gas is satisfactorily supplied to the collecting pipe 14 connected to the other adapter 64 without blocking the passage of the cleaning gas from the supply pipe 36 to the partial adapter 64 in the branch path. Therefore, the change in the amount of the cleaning gas passing through the collection pipe 14 due to the number of collection pipes 14 connected to the adapter 64 can be reduced (see FIG. 5).

  Further, the amount of the cleaning gas passing through the collection pipe 14 is controlled by changing the supply pressure of the cleaning gas by the pressure adjusting valve 42. For this reason, it is not necessary to separately install a flow meter or the like in each branch path from the supply pipe 36 to each adapter 64, and contamination of the cleaning gas by the flow meter or the like can be prevented.

  Further, the humidifier 28 can be connected to the caulking type adapter 64A or the syringe needle type adapter 64B, and the caulking type adapter 64A can be connected to the straight pipe collecting tube 14A, and the syringe needle type. A rubber seal collecting tube 14B can be connected to the adapter 64B.

  Further, a plurality of types of straight tube collection tubes 14A having different outer diameters can be connected to the caulking type adapter 64A, and a plurality of types of rubber seal collection tubes 14B having different outer diameters are connected to the syringe needle type adapter 64B. Made possible.

  In addition, a plurality of types of heating tubes 76 having the same outer diameter and different inner diameters can be attached to the heating furnace 74, and the heating tube 76 attached to the heating furnace 74 is disposed outside the collecting tube 14 to be accommodated. The inner diameter is larger than the diameter by a predetermined length (for example, 1 mm or more and 4 mm or less) so that heat can be efficiently transferred from the heater surface 76A (inner peripheral surface) to the collecting tube 14.

  As described above, a plurality of types of collection tubes 14 having different methods and outer diameters can be aged simultaneously and effectively.

  Further, when the collection tube 14 is slid forward by the forward slide of the fixture 24 and accommodated in the heating tube 76 of the heating furnace 74, the support of the collection tube 14 by the guide 30 is maintained. The drooping of the collection tube 14 is prevented. For this reason, the collection tube 14 can be easily accommodated in the heating tube 76.

  A plurality of main heaters 90 are provided in the heating furnace 74 to reduce the heater capacity (heat generation capacity) of each main heater 90, and a heat storage material 96 is provided in the heating furnace 74 to store heat in the heating furnace 74. The capacity has been increased. For this reason, even if the temperature in the heating furnace 74 falls instantaneously from the set temperature immediately after the collection tube 14 is accommodated in the heating furnace 74, the number of the collection tubes 14 accommodated in the heating furnace 74. Even if the temperature falls within the heating furnace 74 and the amount of instantaneous decrease from the set temperature differs, the temperature controller 84 controls the power supply to the main heater 90 while stopping the power supply to the sub heater 92. Thus, a rapid temperature rise in the heating furnace 74 can be prevented. For this reason, the temperature in the heating furnace 74 can be stabilized at the set temperature with a simple structure. Thereby, it can suppress that the collection agent 12 (for example, resin) deteriorates by the overheating (overshoot) of the collection tube 14, and the decomposition product of the collection agent 12 generate | occur | produces, and the aged collection tube 14 can be suppressed. It is possible to suppress the occurrence of a so-called ghost peak at the time of reuse.

  In addition to the main heater 90, a sub-heater 92 is provided in the heating furnace 74. Therefore, when the temperature in the heating furnace 74 is significantly lower than the set temperature (for example, immediately after the power switch 86 is turned on), the temperature control unit 84 supplies power to the main heater 90 and the sub heater 92. In this case, when the temperature in the heating furnace 74 approaches the set temperature (before reaching the set temperature), the temperature control unit 84 stops supplying power to the sub heater 92 and supplies power only to the main heater 90. Thus, the temperature in the heating furnace 74 is prevented from exceeding the set temperature, and the temperature control unit 84 controls the power supply to the main heater 90 while maintaining the stop of the power supply to the sub heater 92. The temperature in the heating furnace 74 is maintained at the set temperature (see the solid line A in FIG. 11). Accordingly, when the temperature control unit 84 supplies power only to the main heater 90 when the temperature in the heating furnace 74 is significantly lower than the set temperature while maintaining the effect that the heating furnace 74 has a simple structure ( Compared to the broken line B in FIG. 11, the temperature in the heating furnace 74 can be set to the set temperature in a short time (rapidly).

  Further, in the storage container 44 of the humidifier 28, the cleaning gas permeates the liquid retaining portion 56 in which the humidifying agent is held, so that the humidifying agent is made fine particles by the cleaning gas and released to the space layer 60. The moisturizing agent particles that have passed through the space layer 60 pass through the liquid stopping part 62, so that they have a uniform optimum particle shape and are discharged to the front side of the liquid stopping part 62 in a colorless and transparent state. Therefore, the cleaning gas can be appropriately humidified with a simple configuration, and the sample gas can be favorably desorbed from the collection agent 12 in the collection tube 14. As a result, it is possible to prevent a ghost peak from occurring due to a background (residual component) to the collection agent 12 during aging when the aged collection tube 14 is reused, and excessively dispose the collection tube 14 during aging. It is not necessary to heat, and deterioration of the collection tube 14 (collection agent 12) can be prevented.

  By the way, in the aging device 10, if the amount of the humidifying agent retained in the cleaning gas is large, the collecting agent 12 in the collecting tube 14 is damaged, or the humidifying agent stays in the collecting tube 14 after aging. The background to the collection agent 12 is not decreased because of the occurrence of contamination and contamination due to the contamination. For this reason, it is preferable that the retention amount of the humidifying agent in the cleaning gas is very small, and the humidified cleaning gas is allowed to pass through the collection tube 14 and then the continuously dried cleaning gas is allowed to pass therethrough. Is preferred.

In the humidifier 28, when the supply amount of the cleaning gas is 50 mL / min, the humidification time of the cleaning gas is 1 hour, the temperature of the cleaning gas is 20 ° C., and the relative humidity of the cleaning gas is 100% RH, the cleaning gas The absolute humidity is 14.82 g / Kg. Assuming that the cleaning gas is 1 L / g air, the retention amount of the humidifying agent in the cleaning gas is
14.82 g / (1000 L / (50 mL × 60 min)) = 0.044 g
It becomes.

  For this reason, the retention amount of the humidifying agent in the cleaning gas is extremely small, and the humidification method in which the relative humidity of the cleaning gas is not allowed to exceed 100% RH as in the humidifier 28 is optimal for the aging device 10. .

  Further, the partition wall 48 seals the injection port 46 of the storage container 44 of the humidifier 28, and the humidifier retains the liquid via the injection tube in a state where the injection tube of the syringe-like injector penetrates the partition wall 48. It is injected into the part 56. For this reason, a humidifier can be easily inject | poured into the liquid retention part 56. FIG.

  Moreover, before the collection tube 14 is aged, the above-mentioned minute amount of the humidifying agent measured by the injector is injected into the liquid retention unit 56, and when the collection tube 14 is aged, the liquid retention unit 56 is injected. Even after the humidifier is not retained, the cleaning gas is supplied into the collection tube 14 via the humidifier 28. For this reason, the cleaning gas dried after passing the humidified cleaning gas through the collection tube 14 can be easily passed.

  Furthermore, as shown in FIG. 7, when the collection tube 14 is aged, the relative humidity of the cleaning gas is kept constant while the humidifying agent is held in the liquid retaining unit 56, and the humidifying agent is retained in the liquid retaining unit 56. The relative humidity of the cleaning gas is drastically reduced at the stage when the gas is no longer maintained. Therefore, no special operation is required from the step of passing the cleaning gas humidified at a constant humidity into the collection tube 14 (simply passing the cleaning gas continuously into the collection tube 14) and smoothly. It is possible to quickly move to the step of passing the dried cleaning gas through the collection tube 14 (without gradually decreasing the humidity of the cleaning gas).

  In the present embodiment, the collection tube 14 connected to the humidifier 28 via the adapter 64 is supported by the guide 30 to prevent the collection tube 14 from hanging down. It is good also as a structure which can prevent drooping of the collection pipe 14 without the guide 30 by making the attachment strength of the adapter 64 and the connection strength of the collection pipe 14 to the adapter 64 high.

  Furthermore, in the present embodiment, the orifice 50 is provided in the humidifier 28, but the orifice 50 may be provided in the branch pipe 32.

  Moreover, you may use the aging apparatus 10 in this Embodiment as a volatilization apparatus for the analysis of sample gas (a behavioral analysis of a volatile component is included). In this case, for example, as shown in FIG. 12, a sample 98 as a sample body is held in the collection tube 14 instead of the collection agent 12, and the collection tube 14 is lengthened and accommodated in the heating furnace 74. At this time, the discharge port 70 protrudes forward from the heating furnace 74. A collection tube (not shown) may be attached to the discharge port 70 of the collection tube 14. Accordingly, the sample gas (volatile component) generated from the sample 98 and discharged from the discharge port 70 is subjected to sensory evaluation (odor evaluation) by a person every time, or directly or in the collection tube 14 (inside It is possible to indirectly introduce it into a gas chromatograph using a material in which the collecting agent 12 is retained) or the like for analysis.

It is the side view seen from the left which shows the aging apparatus which concerns on embodiment of this invention. It is the top view seen from the upper side which shows the aging apparatus based on embodiment of this invention. It is the side view seen from the left which shows the state which accommodated the collection pipe | tube in the heating furnace in the aging apparatus which concerns on embodiment of this invention. It is a schematic diagram which shows the supply condition of the cleaning gas to the several collection pipe | tube in the aging apparatus which concerns on embodiment of this invention. It is a graph which shows the supply resistance of the cleaning gas to the adapter to which the collection pipe is connected and the adapter to which the collection pipe is not connected in the aging device according to the embodiment of the present invention. It is sectional drawing seen from the left which shows the humidifier in the aging apparatus which concerns on embodiment of this invention. It is a graph which shows the relationship between the humidification time (elapsed time) of the cleaning gas and the humidity (relative humidity) of the cleaning gas in the aging device according to the embodiment of the present invention. It is the side view seen from the left which shows the connection aspect of the humidifier in the aging apparatus which concerns on embodiment of this invention, an adapter, and a collection pipe. (A) thru | or (D) are sectional drawings which show the various heating tubes attached to the heating furnace in the aging apparatus which concerns on embodiment of this invention. It is a schematic diagram which shows the heating furnace etc. in the aging apparatus which concerns on embodiment of this invention. It is a graph which shows the relationship between the temperature in the heating furnace in the aging apparatus which concerns on embodiment of this invention, and the elapsed time (hour) from the heating start in a heating furnace, and the continuous line A is a heating furnace by a main heater and a sub heater. The case where the inside is heated is shown, and the broken line B shows the case where the inside of the heating furnace is heated only by the main heater. It is the side view seen from the left which shows the condition which uses the aging apparatus which concerns on embodiment of this invention as a volatilization apparatus.

Explanation of symbols

10 Aging device (discharge device)
12 Collection agent (sample)
14 Collection tube (sample container)
28 Humidifier (supplying means, branching section, humidifying means)
30 Guide (Guiding means)
32 Branch pipe (supply means, branch section)
34 Resistance tube (supply means, branching section, resistance means)
36 Supply pipe (supply means)
44 Container 46 Inlet 48 Bulkhead (sealed part)
50 Orifice (resistance means)
56 Liquid retention part 60 Spatial layer (space part)
62 Liquid stoppage (release part)
64 adapter (supply means, branching section, connection means)
74 Heating furnace (heating means)
76 Heating tube (heating vessel)
90 Main heater (heating element)
92 Sub-heater (additional heating element)
98 Sample (sample body)

Claims (11)

A sample body from which the sample gas is desorbed by being heated is connected to a sample container provided therein, and a supply means for supplying a supply gas into the sample container;
Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
A liquid holding part that is provided in the supply unit and that holds liquid and allows a supply gas to permeate; a space part that is disposed on the sample container side of the liquid holding part; and a liquid container part on the sample container side of the space part. A humidifying means having a discharge part arranged and discharged from the liquid holding part through the space part into particles and discharged to the sample container side together with a supply gas;
Ejector equipped with. The humidifying means is
A storage container for storing the liquid-retaining part and provided with an inlet;
A sealing portion provided so as to seal the injection port, and capable of injecting liquid into the liquid retaining portion;
The discharging apparatus according to claim 1, comprising:   3. The discharge device according to claim 1, wherein the supply unit supplies the supply gas into the sample container even after the liquid is no longer held in the liquid holding unit. A sample body from which the sample gas is desorbed by being heated is connected to a sample container provided therein, and a supply means for supplying a supply gas into the sample container;
Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
Guiding means for supporting the sample container and guiding the arrangement of the sample container to the heating means;
Ejector equipped with.   5. The supply means is capable of simultaneously supplying a supply gas into the plurality of sample containers, and the heating means is capable of simultaneously heating the plurality of sample containers. Discharge device. A sample body from which the sample gas is desorbed by being heated is connected to a sample container provided therein, and a supply means for supplying a supply gas into the sample container;
A heating means that has a plurality of heat generating portions that generate heat, and desorbs the sample gas from the sample body by heating the sample container, and discharges the sample gas from the sample container;
Ejector equipped with.   The discharge device according to claim 6, further comprising an additional heat generating portion that is provided in the heating unit and generates heat when the heating temperature of the heating unit is increased. A sample body from which the sample gas is desorbed by being heated has a plurality of branch portions connected to each of the plurality of sample containers provided therein, and a supply means for supplying a supply gas into the sample container; ,
A plurality of resistance means provided at each of the plurality of branch portions and imparting resistance to the supply gas passing through the branch portions;
Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
A discharge device characterized by that. A connecting means connected to a sample container in which a sample body from which the sample gas is desorbed by heating is provided, and a supply means for supplying a supply gas into the sample container;
Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
With
A plurality of types of sample containers can be exchanged and connected to the connection means.
A discharge device characterized by that. A connecting means connected to a sample container in which a sample body from which the sample gas is desorbed by heating is provided, and a supply means for supplying a supply gas into the sample container;
Heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
With
A plurality of types of the connection means having different types of connectable sample containers can be replaced and installed in the supply means.
A discharge device characterized by that. A sample body from which the sample gas is desorbed by being heated is connected to a sample container provided therein, and a supply means for supplying a supply gas into the sample container;
A heating means to which the sample container is accommodated, heating means for desorbing the sample gas from the sample body by heating the sample container and discharging the sample gas from the sample container;
With
A plurality of types of the heating containers having different types of the sample containers that can be accommodated can be attached to the heating means.
A discharge device characterized by that.

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