JP6068251B2 - Headspace sample introduction apparatus and method - Google Patents

Description

  The present invention introduces a sample into an apparatus such as a gas chromatograph (GC) or a gas chromatograph / mass spectrometer (GC / MS), and separates and analyzes the sample. The present invention relates to a head space sample introduction apparatus and method for collecting by a space method and introducing the sample into an apparatus such as GC or GC / MS.

  In the headspace sample introduction method, a liquid sample or a solid sample contained in a glass container is heated at a predetermined temperature for a predetermined time to volatilize a volatile component, and a gas containing the volatile component from an upper space (so-called headspace) in the container. A part of the sample is collected and introduced into an apparatus such as a gas chromatograph (GC) or a gas chromatograph / mass spectrometer (GC / MS) for sample separation and analysis. Such sample introduction methods are widely used for water quality analysis, food analysis, material analysis, residual organic solvent analysis in chemicals, forensic analysis and the like.

  What is important in the headspace sample introduction method is how quickly the volatile component of the sample is obtained from the liquid or solid sample. For this reason, the component is rapidly volatilized and collected in a sealed container. Therefore, efficient heating and stirring of the sample are required.

  As such a head space sample introduction device, for example, US Pat. No. 6,168,759 (Patent Document 1) and Japanese Patent No. 3775008 (Patent Document 2) are provided with a sample bottle holding hole in a metal platen, A sample bottle containing the sample is placed in the sample bottle holding hole, and the metal platen is heated by a heater to achieve gas-liquid equilibrium in the sample bottle, and the volatile components in the sample in the sample bottle are volatilized. There has been proposed an apparatus for sucking volatile components in a sample bottle by needle insertion. In the apparatus of Patent Document 2, a device is added to make the sample bottle heating uniform by filling the sample bottle holding hole with a heat medium liquid such as oil.

  Also, for example, in US Pat. No. 5,441,700 (Patent Document 3), a plurality of sample bottles are installed radially in the heating section with respect to the rotation axis, the sample bottles are rotated horizontally, and the sample is placed on the inner wall of the sample bottle. A device that generates volatile components by heating while contacting them and realizes a vapor-liquid equilibrium state, and then sucks the volatile components from the headspace by pushing a needle into the cap provided at the sample bottle mouth with a solenoid plunger. Has been proposed.

US Pat. No. 6,168,759 Japanese Patent No. 3775008 US Pat. No. 5,441,700 JP 2011-203117 A

  As described above, it is understood that in the headspace sample introduction method, it is important to heat the sample liquid at a predetermined temperature in order to volatilize volatile components from the sample and obtain a gas-liquid equilibrium state at an early stage. .

  When using the metal platen used in Patent Document 1 or the like, the sample glass bottle housed in the chamber is heated by heat conduction by a cartridge heater installed near the central axis. However, the platen itself has a large heat capacity, and requires a large amount of energy for the heater that heats the platen and the drive unit that drives the platen, and the heating takes time. Also, when optimizing the analysis conditions, it may be necessary to change the temperature of the sample in the sample container, and it takes too much time to control the temperature of the sample through the platen, which is not practical. .

  In addition, in the apparatus and method for heating the sample container in the metal platen holding hole, an appropriate gap is required between the sample container and the holding hole for smooth insertion and removal of the sample container. It is. Due to this gap, there is a gap between the sample container and the holding hole depending on the location, and there may be a partial difference in the degree of contact between the holding hole and the sample container. Only heating by reflected heat is required, and it is difficult to efficiently and uniformly heat the sample container and the sample.

  In addition, as in Patent Document 2, in a device and method for heating a sample container holding hole provided in a metal platen by filling it with a heat medium liquid such as oil, a heating medium liquid circulation mechanism, a temperature control device, Measuring devices and mechanisms for the management of the heat transfer liquid are required, the overall structure is complicated, a mechanism for wiping the heat transfer liquid is required, and the sample container must be cleaned during analysis. In addition, there is a drawback that it is difficult to maintain and manage the needle, and a needle installed above the sample container is exposed to the heat medium vapor at the time of temperature change, which causes a problem in analysis due to contamination.

  In addition, the apparatus disclosed in Patent Document 4 discloses a mechanism in the headspace gas sampler that stirs air using a fan when heating the oven in which the sample container is stored, so that the temperature in the oven is not uneven. Has been. However, in this structure, since a propeller fan is used, the blowing of air is limited upward or downward, and heat exchange cannot be performed by directly blowing air to the surrounding sample container. The heating effect is limited, for example, the heating effect cannot be obtained unless the number of rotations of the fan is increased, and furthermore, the temperature of the entire heating unit is lowered due to the feeding of the sample container, so that the temperature control of the sample is extremely difficult.

  Therefore, in the present invention, in order to perform heating and temperature control of the sample in a short time, circulation of the heated air in the oven is forcibly and quickly performed, the heating rate is fast, the warm-up time is shortened, and the energy saving effect is achieved. The purpose is to obtain. It is another object of the present invention to heat the sample efficiently and uniformly. It is another object of the present invention to simplify the use and management maintenance of the headspace sample introduction device by simplifying the structure. A further object is to enable very efficient headspace sampling. Another object is to facilitate the temperature control of the sample.

  In order to achieve the above object, the present invention can efficiently heat sample containers such as sample vials and sample bottles, can realize rapid gas-liquid equilibrium and solid-liquid equilibrium, and can be optimally heated for sampling headspace samples. The present invention proposes an apparatus for introducing a headspace sample, and the present invention provides a rotary substrate in an oven provided with a heater so as to be rotatable about a rotation axis, and a centrifugal blower above the central portion of the rotary substrate. And a sample container holder is provided on the rotating substrate on the same circumference centered on the rotating shaft.

  In the headspace sample introducing apparatus, the holding portion is formed in a cylindrical shape or a substantially cylindrical shape, and a ventilation portion is provided in the holding portion.

  In the headspace sample introducing apparatus, the ventilation section is constituted by a notch formed in the holding section.

  Further, in the head space sample introducing device, the holding portion is formed of a collection of columnar bodies, and an interval between adjacent columnar bodies is less than a lateral outer diameter of the sample container. It is.

  In the headspace sample introducing apparatus, the holding section is provided in a plural number so as to be opposed to the centrifugal blower outside the centrifugal blower.

  In the headspace sample introduction apparatus, the ventilation section is provided to face the circumferential tangent direction of the centrifugal blower.

  Further, in the head space sample introduction device, the ventilation portion is perpendicular to a center line connecting the center of the rotating substrate and the center of the holding portion and is located on the inner side of the rotating substrate from a front and rear dividing line passing through the center of the holding portion. The head space is characterized in that two are provided on the outer side of the rotating board from the front and rear dividing lines, and two inside the rotating board from the front and rear dividing lines are provided on each side of the center line. It is a sample introduction device.

  In the headspace sample introducing device, the centrifugal blower is a one-side suction type or an upper and lower side suction type of the upper or lower side.

  In the headspace sample introducing apparatus, the heater is installed on an inner side wall of the oven.

  In the headspace sample introduction device, an opening is provided above the sample container in the upper part of the oven, and a needle for collecting a target component is disposed in a continuous space above the opening. This is a headspace sample introduction device.

  In the headspace sample introducing apparatus, the upper end portion of the space is covered with a heating medium.

  In the headspace sample introducing device, the side portion of the space is covered with a shielding material.

  Further, a sample placed on a concentric circumference centered on the centrifugal blower by rotating the centrifugal blower installed in the center of the oven and sucking air heated by the heater from above or below the centrifugal blower A headspace sample introduction method characterized by blowing air to a container.

  In the headspace sample introduction method, the heater is installed on an inner side wall of the oven.

  According to the method and apparatus of the present invention, the circulation of the heated air in the oven is forced and sucked by using a centrifugal blower and sucking heated air from the top or bottom of the fan and blowing it out in the circumferential tangential direction. Even when the heater capacity is small, the heating rate is fast, the warm-up time is shortened, and the energy saving effect is obtained.

  Furthermore, the heated air is blown in a limited manner in the height direction of the holding part and concentratedly on the holding part to suppress the temperature distribution to a minimum. However, the heated air blown to the holding part enters from the ventilation part of the holding part, wraps and heats the sample container stored in the holding part, exits from the ventilation part on the downstream side of the ventilation, and again after heating by the heater Since the sample is circulated, the heating rate of the sample is extremely fast. As a result, the efficiency of equilibration of the sample in the sample container is increased, the equilibration time and the analysis time are shortened, and the reproducibility of the analysis is obtained.

Flow chart of automatic introduction system flow of one embodiment of the present invention Cross-sectional schematic explanatory diagram of the main part of one embodiment of the present invention The principal part perspective view of one embodiment of the present invention Same as above Example of other part perspective view The main part plane explanatory drawing of one embodiment of the present invention One embodiment of the present invention. One embodiment of the present invention, etc. Operational explanatory diagram of the main part of one embodiment of the present invention Other embodiment of the present invention other part operation state explanatory diagram 1 is a schematic perspective view of an essential part of one embodiment of the present invention. 1 is a schematic perspective view of an essential part of another embodiment of the present invention.

  Hereinafter, the present invention will be described in detail with reference to the drawings. FIG. 2 is a schematic explanatory diagram of the headspace sample introduction apparatus W of the present invention. The head space sample introduction device W includes an oven 1, a rotating substrate 2, a rotating shaft 21, a holding unit 4, a heater 5, a centrifugal blower 6 and other members. Conveniently, the oven 1 is configured such that the case components are combined so that they can be divided at the center, and the overhangs are fixed by a fixing tool such as a screw to be integrated. The oven 1 constitutes a heating part for the sample and the sample container 3 and is covered with a heat insulating material or is made of the heat insulating material itself to provide heat insulation. In addition, although it does not specifically limit as a shape of the whole oven, Since heating air will flow efficiently if the inside is a column shape, heating efficiency increases. If possible, if the entire oven interior is a sphere, the thermal efficiency is further increased. However, in actuality, the oven is formed taking into consideration cost, ease of processing, and the like.

  The rotary substrate 2 is a substrate for installing the holding portions 4, 4,... That hold the sample containers 3, 3, and so on, and is supported by the rotary shaft 21 in the oven 1. A motor 22 that extends through a through-hole 13 provided in the bottom plate 12 and that is provided in the lower portion is rotatably installed via a driving wheel or gears 23 and 24. The sample container 3 is formed in a desired shape by a vial, a glass bottle or the like, but is preferably formed in a cylindrical body.

  As shown in FIGS. 3 and 4, the holding portion 4 is formed by a cylindrical holding member 40, and a vertically long cutout is provided on the side wall thereof to form a ventilation portion 41. Here, since the heated air is blown from the centrifugal blower 6 in the circumferential tangential direction of the centrifugal blower 6, when the ventilation portion 41 is positioned with respect to the direction, the heated air is directly applied to the sample container 3. Therefore, the heating effect of the sample in the sample container 3 is improved. Although the formation form and the number of the ventilation parts 41 are not specifically limited, It is preferable to set it as plural, especially three. And although these three ventilation parts 41, 41, 41 are not specifically limited, it is preferable to form along the axial direction of the cylindrical holding member 40 by arrangement | positioning at intervals of 120 degree | times.

  As shown in FIG. 5, the three ventilation portions 41, 41, 41 formed on the holding member 40 are orthogonal to the center line X connecting the center of the rotating substrate 2 and the center of the holding portion 4 and the holding portion 4. Two are provided inside the rotary substrate 2 from the front and rear dividing lines Y passing through the center, and one is provided outside the rotary substrate 2 from the front and rear dividing lines Y. With such an arrangement, the blown heated air warms the sample container 3 in the holding unit 4 without diffusing from the two ventilation units 41, 41 and is discharged from the remaining one ventilation unit 41. Here, it is useful for improving the heating effect of the sample container 3 that the sample container 3 is continuously heated by the heated air until the air is discharged from the one ventilation portion 41.

  Note that the ventilation portion 41 provided in the holding member 40 is not limited to the above configuration, and a front-rear dividing line Y that is orthogonal to the center line X connecting the center of the rotating substrate 2 and the center of the holding portion 4 and passes through the center of the holding portion 4. Further, a configuration may be adopted in which one is provided inside the rotating substrate 2 and two are provided outside the rotating substrate 2 from the front and rear dividing lines Y.

  As shown in FIG. 3, the upper end of the holding member 40 may be formed to be connected by the connecting portions 43, 43, or as shown in FIG. 4, the upper end of the holding member 40 is opened by a notch. You may make it form. When used over a long period of time, it is assumed that the durability is higher when the upper ends are connected.

  Further, the holding unit 4 has a mechanism for holding the sample container 3 so that the sample container 3 does not fall down during insertion and removal, and heated air can be directly blown from the centrifugal blower 6 to the sample container 3. If so, the present invention is not limited to the above configuration, and a large number of through holes are formed in the cylindrical body to provide ventilation portions, or the cylindrical body is formed by a net-like wall body 49 as shown in FIG. It is also possible to form a large number of ventilation portions 41 on the entire surface of the holding portion, or to arrange several columnar bodies 47, 47... On one circumference as shown in FIG. In this case, the adjacent interval between the columnar bodies 47 is less than the lateral outer diameter of the sample container 3. By doing so, the sample container 3 does not roll over when the sample container 3 is inserted into, removed from, or stirred during heating. Moreover, the raw material of the holding | maintenance part 4 is not specifically limited, If it has heat resistance to about 500 degreeC, it can form with desired materials, such as a metal, ceramics, a ceramic, and a synthetic resin. In particular, if the metal has good heat conduction, the radiant heat from the heated metal is also useful for heating the sample. Actually, ease of processing and cost are considered.

The heater 5 is installed on the bottom 12 or the side wall 19 of the oven 1, the top plate 10, etc. so as to surround the outer periphery of the holding parts 4, 4, 4 of the sample container 3 provided on the rotating substrate 2. Here, it is desirable to make the temperature of the entire sample container 3 uniform in order to vaporize the sample efficiently. For this reason, the heater 5 is preferably positioned at a height that is about half of the sample container 3. Further, in order to correspond to the sample containers 3 having various capacities, the sample containers 3 can be positioned at a height about half of the holding portion 4. As the heater 5, a sheathed heater can be used as an example. For example, the sheathed heater may be formed in an arc shape and may be provided on two or three concentric circles, or the entire holding portions 4, 4, 4 may be provided. It can be formed in a circular shape surrounding it. In addition, by using a ceramic heater having a high heating rate as the heater 5, the sample can be rapidly vaporized. Further, by using a halogen heater as the heater 5, heating that is focused only on the sample to be heated can be performed, and energy-efficient heating can be performed. However, even in these cases, in order to prevent the heating effect from being reduced due to the temperature difference between the sample container 3 and the surroundings, it is desirable that the entire interior of the oven be warmed by blowing air from the center. In any of the above, the sample is heated by double heating, that is, direct heating of the sample from the surrounding heater 5 and heating by blowing the heated air in the centrifugal direction from the center of the oven 1. Is a feature.
In addition, the installation location and the installation method can be appropriately selected by installing a cartridge heater at the center of the rotating substrate 2 or hanging the cartridge heater on the top plate 10 of the oven 1.

  The centrifugal blower 6 may be any blower as long as it blows in the circumferential tangent direction of the blower. As an example, a sirocco fan that is a centrifugal multiblade fan is used. A motor 62 for driving the sirocco fan is connected by a shaft 63 provided through the center of the rotating shaft 21. There are various shapes of this sirocco fan, and each can be used, but a typical example is shown here.

  The sirocco fan is formed by providing a large number of blades and through-holes on the side plate and fixing them to the disc-shaped main plate, providing a rotation shaft hole at the center of the disc-shaped main plate, and inserting and fixing the shaft 63. The sirocco fan may be a single-side suction type from above or below, but an upper and lower side suction type may be used as necessary. The through holes are formed in a vertically long shape, and the blown air is not diffused up and down but concentrated within the height of the holding portion 4. The rotational speed of the fan is not particularly limited, but is preferably about 1000 to 5000 rpm, and 3000 rpm is often used. At 1000 rpm or less, since the wind force is weak, the heating effect of the sample by the heated air is low. In addition, although a heating effect arises even at 5000 rpm or more, the effect does not increase markedly compared with the effect up to 5000 rpm.

  A hole 44 communicating with the opening 24 provided in the rotary substrate 2 is provided at the bottom of the holding unit 4 so that it can pass through an elevator 7 and a needle elevator 105 of the sample container 3 described later.

  The elevator 7 of the sample container 3 removes the sample container 3 from the tray 8 through the opening 24 provided in the rotary substrate 2 and the hole 44 of the holding part 4 through the through hole 131 provided in the bottom part 12 of the oven 1 as described above. 1 is a device for insertion into the device.

  The tray 8 accommodates the sample containers 3, 3... Has a large number of storage holes 81, 81... Concentrically formed around the shaft 83, and is configured to be rotatable by a motor 82 connected to the shaft 83. . As shown in FIGS. 6 and 7, the tray 8 is in contact with the top plate 10 of the oven 1 or the top plate 14 of the head space sample introduction device W, and the top plate 14 is further provided with a through hole 15. Further, a shutter 9 is provided on the top plate 10 above the oven 1 so as to be rotatable by its shaft 91.

  The shutter 9 is configured in two upper and lower stages and covers the through hole 16 of the oven 1 and the through hole 15 of the head space sample introduction device W, respectively, by dropping the sample container 3 from the tray 8 and touching the outside air. The temperature drop in the oven 1 is prevented. When inserting the sample container 3 from the tray 8 into the oven 1, the sample container 3 is allowed to pass through by communicating the through holes 15 and 16 with the through hole 93 of the shutter 9.

  As shown in FIGS. 8 and 9, a sample container heating section opening 11 is formed on the top plate 10 of the oven 1 above the sample container 3 having the target component vaporized by heating in the gas phase. In addition, a space 18 provided with a needle 101 for collecting a target component is provided above the opening 11 continuously with the opening 11 in a state of being blocked from outside air by a heat insulating tube 102. A heating medium is disposed in the upper portion of the space 18. Specifically, a heating plate 104 is installed as a heating medium, and the needle 101 is inserted into the space 18 from the heating plate 104. With this structure, when the air circulates in the oven 1 above or below the centrifugal blower 6, the opening 11 and the space 18 are warmed by the heated air. As a result, the tip of the needle 101 near the opening 11 has substantially the same temperature as in the oven 1. Therefore, the temperature difference between the tip of the needle 101 and the inside of the sample container 3 does not impair the gas-liquid or gas-solid equilibrium and the target component is not denatured.

  As another configuration, when the heating plate 104 is adjacent to the oven 1 without providing the space 18 and the needle 101 is disposed in the oven 1 from the heating plate 104, the tip of the needle 101 is placed in the oven 1. The needle 101 can be set to the set temperature of the heating plate 104.

  On the other hand, since the upper part of the needle 101 is connected to the heating plate 104, the temperature can be the same as that of the heating plate 104. The heating plate 104 is set higher than the oven 1 by about 5 to 30 ° C. From this structure, the tip of the needle 101 can be set close to the temperature of the oven 1, and the upper part of the needle 101 can be set to a temperature close to the heating plate 104. As a result, a cold point does not occur in the needle 101 after collecting the target component, so that there is no problem of adsorption during the introduction of the target component, and the problem of carryover caused thereby. Moreover, the side part of the space 18 where the tip of the needle 101 is installed is covered with a heat insulating tube 102, and the heat insulating tube 102 may be provided with a shielding part 103 made of a heat insulating member or the like.

  Then, the sample container 3 heated or stirred and containing the target component in the gas phase is pushed up by the needle elevator 105, and the sample container 3 is inserted into the space 18. At that time, the needle 101 in the space 18 is stuck in the septum 31 of the sample container 3, and the target component in the gas phase in the sample container 3 is collected. The target component is collected by the needle 101 and then sent to the analyzer or the like through the valve A2 in the heating plate 104 or a conduit.

  The needle elevator 105 is stored in the holding unit 4 through the through hole 24 provided in the rotating substrate 2 and the hole 44 provided in the bottom of the holding unit 4 through the through hole 17 provided in the bottom plate 12 of the oven 1. The sample container 3 is pushed up, and the sample container 3 is joined to the needle 101 installed above the oven 1.

  As shown in FIG. 1, the headspace sample automatic introduction system 100 of the present invention mainly includes a sample weighing unit A in addition to the above-described headspace sample introduction device W provided with a tray 8 and an oven 1 serving as a sample container heating unit. , An interface unit B, a gas control unit C, an electric control unit, a host computer user interface D, and the like.

  The oven 1 includes not only the configuration of the sample container heating section itself, but also means for transferring and mixing the sample container 3. The sample measuring unit A can be heated at a temperature equal to or higher than the predetermined temperature of the needle A1, the 6-way or 8-way injection valve A2.

  The interface part B has a transfer line B1 and can be heated at a temperature equal to or higher than a predetermined temperature of the oven 1. The gas control unit C automatically adjusts the gas flow rate and pressure using an electronic fluid control device C1, a solenoid valve (Press. Valve) C2, a solenoid valve (Vent Valve) C3, a resistor (resistor tube) C4, and the like. . The electric control unit D rotates the tray 8 of the sample container 3, recognizes the sample container 3, transfers the sample container 3, operation and temperature control of the heater 5 as a heating unit of the oven 1, operation and temperature of the sample measuring unit A, interface Controls temperature control of part B, gas flow rate and pressure of gas control part C, etc., set by the user from host computer user interface D, headspace sample automatic introduction system main body, GC (gas chromatograph) and host It is possible to automatically control operations to meet a series of analysis purposes through communication between computers.

  Next, an outline of the flow path and operation of the headspace sample automatic introduction system 100 and the headspace sample introduction apparatus W of the present invention will be described. An analysis sample (liquid or solid sample) is sealed in a sample container 3 such as a sample glass bottle and then stored in a storage hole 81 of a sample container tray 8. The sample container 3 is fed into and held in a holding portion 4 at a predetermined position in the oven 1 by an elevator 7 which is a lifting mechanism for the sample container 3. The sample is heated at a constant temperature for a predetermined time, and the volatile component is driven out into the gas phase by gas-liquid or solid-gas distribution in the sample container 3. If necessary, when the sample container 3 is heated by the means for transferring and mixing the sample container 3, the sample container 3 may be given a three-dimensional vibration such as a vertical direction and a front-rear direction to promote equilibration. Due to this vibration, the target component in the liquid phase moves near the gas phase, or the contact area between the liquid phase and the gas phase increases, so that rapid equilibration can be achieved.

  When volatile components accumulate in the sample container 3, the sample container 3 is positioned on the needle elevator 105 by the rotation of the rotating substrate 2. By raising the needle elevator 105, the sample container 3 is lifted to a predetermined position in the oven 1, and the needle 101 is pierced into the septum 31 of the sample container 3. With the electromagnetic valve C3 closed, a pressurized gas (for example, nitrogen or helium) pressurizes the inside of the sample container 3 via the electromagnetic valve C2. A part of the gas sample including the analysis components present in the sample container 3 flows into the sample measuring tube (sample loop) A3 in a state where the electromagnetic valve C2 is closed and the electromagnetic valve C3 is opened. The 6-way or 8-way injection valve A2 is switched, and the GC or GC / MS carrier gas is adjusted by the GC electronic fluid control unit (GC / EPC) D, passes through the sample loop A3, and the weighed sample is transferred to the transfer line B1. Through and into the GC. Then, the sample is separated and analyzed by GC or GC / MS.

  A rotating substrate 2 is rotatably supported by a rotating shaft 21 in the oven 1. On the rotating substrate 2, six holding members 4, 4... Are installed at equal intervals on the same circumference. The holding member 4 is formed with two ventilation portions 41 at the front and one ventilation portion 41 toward the center of the rotation shaft 21. Each ventilating portion 41 is connected to the upper end by a connecting portion 43. Above the central portion of the rotating substrate 2, the sirocco fan 6 centered on the rotating shaft 21 is supported by the shaft 63, and is rotatably provided by the motor 62 through the hollow of the rotating shaft 21 of the rotating base 2. .

  In the oven 1, a sheathed heater 5 formed in a semicircular shape so as to surround the outer periphery of the holding portions 4, 4, 4 is installed on the side wall 19 of the oven 1. The elevator 7 of the sample container 3 passes through a through hole 131 provided in the bottom portion 12 of the oven 1 and can be freely moved into and out of the holding portion 4 so that the sample container 3 can be pushed up or lowered.

  With the above configuration, the air in the oven 1 is heated by the sheathed heater 5. As the sirocco fan 6 rotates, heated air is sucked from the upper part of the sirocco fan 6, passes through a through hole from the center of the sirocco fan 6, and heated air is regularly blown out in the circumferential tangent direction of the sirocco fan 6.

  The heated air does not diffuse up and down the holding unit 4, but is intensively blown within the height of the holding unit 4, and the sample stored therein through the ventilation units 41 and 41 provided in the holding unit 4 Directly hits the container 3 and wraps the sample container 3 and heats it efficiently. While the sample container 3 is heated, the hot air hitting the sample container 3 uniformly turns around the opposite side and escapes from the rear ventilation part 41, hits the sheathed heater 5 on the outer periphery thereof, reaches the upper side, and is sucked into the sirocco fan 6 again. It repeats the high-speed circulation that is said.

  As a result, the entire sample container 3 to be heated is uniformly wrapped with hot air, and heat exchange is performed efficiently and at high speed. Moreover, even if the room temperature sample container 3 is fed into the oven 1, the temperature of the other sample containers 3 is hardly affected. This is completely different from the case where the temperature of the entire heating unit is directly affected when the sample container 3 at room temperature is fed into the oven 1 as in the case of a propeller fan, resulting in a large temperature drop.

  The centrifugal blower 6 used in this embodiment has a configuration in which sirocco fans 6 are stacked in two stages. The heater is formed in a circular shape using a sheathed heater 5 and is installed so as to surround the outer periphery of the holding portions 4, 4. In the other configuration, side plates having a plurality of blades and through holes are provided on the outer edge of the disk-shaped main plate, and side plates having the same configuration are respectively installed.

  With this configuration, when the sirocco fan 6 is rotated, heated air is blown into the upper side plate from above, and heated air is blown into the lower side plate from below, with the disc-shaped main plate as a boundary. The heated air is blown out tangentially along the blade from the hole, and the inside of the oven 1 is heated evenly.

By simplifying the structure of the member and the part that holds and heats the sample, the sample container can be heated very efficiently by blowing with a blower, and so-called headspace sample introduction can be performed very efficiently. .
For this reason, extraction of a liquid containing a volatile component from a chemical sample and further supplying it to various analytical instruments has been performed extremely smoothly.
Therefore, it can contribute to water quality analysis, atmospheric analysis, sample analysis, and residual organic solvent analysis in chemicals.

W Headspace Sample Introduction Apparatus 1 Oven 100 Headspace Sample Automatic Introduction System 2 Rotating Substrate 21 Rotating Shaft 23 Driving Wheel 24 Gear 3 Sample Container 4 Holding Part 40 Holding Member 41 Ventilation Part 5 Heater 6 Centrifugal Blower 63 Through-hole 7 Elevator 8 Tray 9 Shutter 105 Needle elevator

Claims (13)

  In the oven in which the heater is installed, the rotating substrate is installed so as to be rotatable around the rotation axis, and a centrifugal blower is installed above the central portion of the rotating substrate, and the rotating shaft is centered on the rotating substrate. A headspace sample introduction device characterized in that a sample container holding portion is provided on the same circumference.   The head space sample introduction device according to claim 1, wherein the holding portion is formed in a cylindrical shape or a substantially cylindrical shape, and a ventilation portion is provided in the holding portion. The head space sample introducing device according to claim 2, wherein the ventilation portion is configured by a notch portion formed in the holding portion.   The headspace sample introduction device according to claim 1, wherein the holding portion is formed of a collection of columnar bodies, and an interval between adjacent columnar bodies is less than a lateral outer diameter of the sample container. The head space sample introduction device according to claim 2 or 3, wherein the ventilation section is provided so as to oppose the circumferential tangent direction of the centrifugal blower.   The ventilation section is perpendicular to the center line connecting the center of the rotating board and the center of the holding section, and two inside the rotating board from the front and rear dividing lines passing through the center of the holding section, and the rotating board from the front and rear dividing lines. 4. The headspace sample introduction according to claim 2, wherein one is provided on the outer side of the substrate and two on the inner side of the rotating substrate from the front and rear dividing lines are provided on each side of the center line. apparatus.   The head space sample introduction device according to any one of claims 1 to 6, wherein the centrifugal blower is an upper or lower one-suction type or an upper and lower both-side suction type.   The head space sample introduction device according to any one of claims 1 to 6, wherein the heater is installed on an inner side wall of the oven.   9. The headspace sample according to claim 8, wherein an opening is provided above the sample container in the upper part of the oven, and a needle for collecting a target component is disposed in a space continuous above the opening. Introduction device.   The head space sample introduction device according to claim 9, wherein an upper end portion of the space is covered with a heating medium.   The headspace sample introduction device according to claim 9 or 10, wherein a side portion of the space is covered with a shielding material.   Rotate the centrifugal blower installed in the center of the oven, suck the air heated by the heater from above or below the centrifugal blower, and place it on the sample container arranged on the concentric circumference centering on the centrifugal blower A method of introducing a head space sample, characterized by blowing air.   The headspace sample introduction method according to claim 12, wherein the heater is installed on an inner side wall of the oven.

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