JP6084838B2 - Test tube reflux device - Google Patents

Description

  The present invention relates to a test tube reflux apparatus for heating and refluxing a test object in a test tube and then cooling the test object.

  A synthesis experiment automation system for conducting a synthesis experiment by putting a solvent in a plurality of synthesis reaction vessels is disclosed in Patent Document 1. This synthesis experiment automation system takes out a synthesis reaction container from a reaction container rack, transports the synthesis reaction container to a dispensing / dispensing device, and at the position of a temperature control unit that reacts under pre-specified experimental conditions of the reaction device. Has a robot to transport. A cooling tower is provided in the upper part of the synthesis reaction vessel, and this cooling tower can cool the hot gas flowing from the synthesis reaction vessel.

JP 2006-015269 A

  In the synthetic experiment automation system described in Patent Document 1 described above, various experiments performed by a researcher can be performed simultaneously, and the system can be easily improved and expanded. However, this synthesis experiment automation system has a complicated system structure, and each of the plurality of synthesis reaction vessels must be provided with a cooling tower, which is large and expensive.

  The present invention has been made in view of the above, and the object of the present invention is to reduce the cost by simplifying the structure, and after simultaneously heating test objects in a plurality of test tubes, An object of the present invention is to provide a test tube reflux device capable of simultaneously cooling test objects in a plurality of test tubes.

In order to achieve the above object, a test tube reflux apparatus according to claim 1 is a test tube reflux apparatus for heating and refluxing a solvent accommodated in a plurality of test tubes and then cooling the test tube. And a heating unit disposed in the main body unit and heating the solvent in the plurality of test tubes at the same time, and disposed above the heating unit, and heated by passing cooling air A cooling unit for simultaneously cooling the solvent in the plurality of test tubes, and a heat unit disposed between the heating unit and the cooling unit to cut off heat of the heating unit, and the solvent in the plurality of test tubes A heat insulating member having a through hole for passing the plurality of test tubes when heated by the heating unit, and the heat insulating member simultaneously causes the solvent in the plurality of test tubes to pass through the cooling unit. When cooling, the plurality of test tubes and the heating unit A plurality of test tubes are passed through the through holes of the heat insulating member when the plurality of test tubes are heated by the heating unit, and the plurality of test tubes are formed by the cooling unit. When the test tube is cooled, the heat insulating member is interposed between the heating unit and the cooling unit in order to block the plurality of test tubes and the heating unit by the blocking region portion of the heat insulating member. Slidably arranged.

In the test tube reflux apparatus according to claim 1, the heating unit can simultaneously heat the solvent in the plurality of test tubes passed through the through holes of the heat insulating member, and in the state where the heat of the heating unit is blocked by the heat insulating member, Can simultaneously cool the solvent in a plurality of heated test tubes. As a result, the structure can be simplified and the cost can be reduced. After simultaneously heating the test objects in the plurality of test tubes, the solvent in the plurality of test tubes can be cooled at the same time.
In addition , when a plurality of test tubes are heated by the heating unit simply by sliding the heat insulating member, a plurality of test tubes are passed through the through holes of the heat insulating member, and when a plurality of test tubes are cooled by the cooling unit, heat insulation is performed. Since the plurality of test tubes and the heating unit can be blocked by the blocking region portion of the member, the structure can be simplified and the cost can be reduced.

In the test tube reflux apparatus according to claim 2 , the width of the blocking region portion of the heat insulating member is equal to or greater than the diameter of the through hole of the heat insulating member.

In the test tube reflux apparatus according to claim 2 , when the test tube is cooled, the shut-off region portion of the heat insulating member can support the test tube, and the heat of the heating portion is cooled by the shut-off region portion of the heat insulating member. It can be insulated so that it does not reach.

In the test tube reflux apparatus according to claim 3 , an arrangement direction of the plurality of test tubes in the cooling unit is deviated from a flow direction of the cooling air passing through the cooling unit.

In the test tube reflux apparatus according to claim 3 , it is possible to prevent the cooling air from directly hitting the test tube, to reduce the temperature difference between the windward side and the leeward side of the test tube, and to reduce the vortex flow of the cooling air. By preventing the generation as much as possible, the airflow loss (resistance) in the cooling section can be reduced.

The test tube reflux apparatus according to claim 4 further includes an elevating part that elevates and lowers the plurality of test tubes with respect to the cooling part and the through hole of the heat insulating member so as to be inserted and removed.

In the test tube reflux apparatus according to the fourth aspect , since the plurality of test tubes can be attached / detached at the same time, the attachment / detachment and replacement of the plurality of test tubes can be facilitated.

  According to the present invention, it is possible to reduce the cost by simplifying the structure, and to provide a test tube reflux device capable of simultaneously cooling after putting test objects in a plurality of test tubes and heating them simultaneously it can.

It is a front view which shows embodiment of the test-tube reflux apparatus of this invention. It is a top view which shows the test tube reflux apparatus of FIG. It is a side view which shows the test-tube reflux apparatus of FIG. It is a figure which shows the cooling box of a test tube heating-cooling part, a heating part, and the example of a shape of a heat insulation member. It is a perspective view which shows the structural example of the cooling box shown in FIG. It is a top view of the cooling box shown in FIG. It is a figure which shows a mode that the heat insulation member of a test tube heating / cooling part is slid. It is a figure which shows the state which lifted the raising / lowering handle to R2 direction, and lifted all the test tubes T up from the heat insulation member simultaneously with the raising / lowering stand. It is a figure which shows the state which inserted the whole solvent M of the lower end part of all the test tubes T in the hole of the electric heater of a heating part. It is a figure which shows the state which lifted the raising / lowering handle in the R2 direction, and the raising / lowering stand lifted all the test tubes T to the Z2 direction at once. It is a figure which shows the state which lowered the raising / lowering handle to the R1 direction, and spaced apart the raising / lowering stand and the flange FF of the upper end part of the test tube T. FIG. FIG. 12A is a conceptual diagram showing a state in which the solvent in the test tube T is heated and refluxed, and FIG. 12B shows a state in which the solvent in the test tube T is cooled. It is a conceptual diagram. It is a figure which shows the example of the experimental data of the recovery after refluxing for 45 minutes, when the solvent M is ethanol water. It is a figure which shows the comparative example of the cooling method and shows the temperature change etc. at the time of cooling.

  DESCRIPTION OF EMBODIMENTS Hereinafter, embodiments for carrying out the present invention (hereinafter referred to as embodiments) will be described with reference to the drawings.

  FIG. 1 is a front view showing an embodiment of the test tube reflux apparatus of the present invention, and FIG. 2 is a plan view showing the test tube reflux apparatus of FIG. FIG. 3 is a side view showing the test tube reflux apparatus of FIG.

  As shown in FIG. 1 and FIG. 2, the test tube reflux apparatus 1 includes a plurality of test tubes T that are detachably mounted, and a solvent M that is a test object accommodated in the plurality of test tubes T. Are simultaneously used (heated), and then the solvent M in the plurality of test tubes T is simultaneously cooled using cooling air, for example, the apparatus used to heat and reflux the solvent M. . In the test tube reflux apparatus 1, for example, the solvent M is alcohol, and the test tube reflux apparatus 1 is used as a sample processing (reaction) apparatus before analysis, but is not particularly limited thereto.

  As shown in FIG. 2, the test tube reflux apparatus 1 includes a main body portion 2, a test tube heating / cooling portion 3 disposed in the main body portion 2, an air supply portion 4, an operation panel portion 5, and a blower device 6. have. As shown in FIGS. 1 and 3, the test tube reflux apparatus 1 further includes a test tube elevating unit 7.

  As shown in FIG. 2, the main body 2 of the test tube reflux apparatus 1 has a rectangular shape when viewed from above, and on the main body 2, the test tube heating / cooling unit 3, the air supply unit 4, and the operation A panel unit 5 is arranged. Although the structure of the test tube heating / cooling unit 3 will be described in detail later, the test tube heating / cooling unit 3 is configured such that a plurality of test tubes T can be detachably provided in a matrix along the X and Y directions. Can be set.

  As shown in FIG. 2, in the illustrated example, as the number of the plurality of test tubes T, for the sake of simplifying the drawing, five in the X direction and five in the Y direction are arranged in a total of 25. In practice, however, any number can be selected, such as 15 in the X direction and 10 in the Y direction, or 20 in the X direction and 20 in the Y direction.

  As shown in FIG. 2, the air supply unit 4 includes a plurality of air hoses 4A and an air hose branch pipe 4B. In the example shown in FIG. 2, five air hoses 4A are prepared, the blowing tip 4C of each air hose 4A reaches the test tube heating / cooling section 3, and the terminal portion 4D of each air hose 4A is an air hose branch pipe. It is connected to 4B. Cooling air AR generated by the blower device 6 serving as an air supply source is supplied to the air hole branch pipe 4B through a duct hose (not shown). The cooling air AR is supplied to the test tube heating / cooling unit 3 side through the five air hoses 4A.

  In the operation panel unit 5 shown in FIG. 2, a temperature controller 5A, an off timer 5B, a timer start switch 5C, and an overheat protector 5D are arranged, and a power cord 5E is connected. The power cord 5E is connected to an AC 100V commercial AC power source. A blower switch 5F is disposed on the switch mounting portion 5G. As shown in FIG. 3, a power switch 5 </ b> H is disposed on the side surface of the operation panel unit 5.

  Next, the test tube heating / cooling unit 3 disposed in the main body 2 will be described.

  The test tube heating / cooling unit 3 shown in FIGS. 1 to 3 includes a cooling box 10, a heating unit 11, and a heat insulating member 12. As shown in FIGS. 1 and 3, the heating unit 11 is held by the holding unit 2 </ b> A of the main body unit 2. The heating unit 11 is an aluminum block having good thermal conductivity, for example. On the upper side of the heating part 11, there is a hole part 11H for inserting the lower end part of each test tube T.

  The cooling box 10 shown in FIGS. 1 to 3 is an example of a cooling unit, and is held above the heating unit 11 in parallel in the Z direction (vertical direction) with an interval. The Z direction, the X direction, and the Y direction are orthogonal to each other.

  FIG. 4 is a perspective view showing a shape example of the cooling box 10, the heating unit 11, and the heat insulating member 12 of the test tube heating / cooling unit 3. FIG. 5 is a perspective view showing a structural example of the cooling box 10 shown in FIG. FIG. 6 is a plan view of the cooling box 10 shown in FIG.

  The heating unit 11 shown in FIGS. 1 and 3 has an electric heater such as a heating wire that generates heat from the power source supplied from the power cord 5E shown in FIG. The heating unit 11 is a rectangular parallelepiped member as shown in FIG. As described above, as shown in FIGS. 1 and 3, a plurality of holes 11 </ b> H are formed in the upper portion of the heating unit 11 at positions corresponding to the number of the plurality of test tubes T. The lower end portions of the test tubes T at corresponding positions are inserted into these hole portions 11H.

  The heating unit 11 shown in FIG. 2 can set the heating temperature by the temperature controller 5A. The time for the heating unit 11 to heat the test tube T can be set by operating the timer by turning on the timer start switch 5C shown in FIG. The overheat preventer 5D illustrated in FIG. 2 prevents the heating unit 11 from overheating. The heating temperature of the heating unit 11 made of aluminum block is preferably 85 ° C. to 90 ° C. on the lower side and 115 ° C. to 120 ° C. on the upper side. The numerical value of the heating temperature of the heating unit 11 can be set to plus 10 ° C. to 20 ° C. with respect to the boiling point of the solvent M to be refluxed.

  As shown in FIG. 4, the cooling box 10 shown in FIG. 5 is held at the top of the heating unit 10 away from the heating unit 10 in the Z direction. The cooling box 10 can be set to be detachable with a plurality of test tubes T detachably spaced in a matrix along the X and Y directions. The cooling box 10 is made, for example, by molding an aluminum plate member having good thermal conductivity.

  The cooling box 10 has a plurality of holding holes 13 for inserting and holding the test tubes T so that they can be inserted and removed. In the illustrated example, the plurality of holding hole portions 13 are formed at intervals in the X direction and are formed in five rows at intervals in the Y direction, and the cooling box 10 is provided for simplification of the drawing. 5 × 5 rows = 25 holding hole portions 13 are provided.

  As shown in FIGS. 5 and 6, the cooling box 10 is divided into five air guides 14. Each air guide portion 14 is formed along the Y direction, and each air guide portion 14 has five holding hole portions 13. Each air guide 14 has a cooling air supply port 15 and a cooling air discharge port 16. The air supply port 15 for cooling is provided with a blowing tip 4C of the air hose 4A. As a result, the cooling air AR enters the cooling air supply port 15 from the blowing tip 4C of the air hose 4A, flows in the air guide portions 14 along the Y1 direction, and removes the solvent M in the test tube T. The air can be cooled and discharged from the cooling air discharge port 16.

  As shown in FIG. 6, in each air guide portion 14, the array line K of the five holding hole portions 13 is on the one wall surface (the left wall surface in FIG. 6) 17 side in the width direction W of the air guide portion 14. It is biased to. As a result, the cooling air AR enters the cooling air supply port 15 from the blowing tip 4C of the air hose 4A, flows in the air guide portions 14 along the Y1 direction, and removes the solvent M in the test tube T. When cooling and discharging from the cooling air discharge port 16, the cooling air AR does not directly hit the test tube T. Thus, in the cooling box 10, since the test tubes T are displaced in the air guide portions 14, the cooling air AR is prevented from directly hitting the test tubes T, and the test tubes T The temperature difference between the windward side and the leeward side of T can be reduced, and the generation of vortex of the cooling air AR can be prevented as much as possible, so that the airflow loss (resistance) in the cooling box 10 can be reduced.

  The plurality of test tubes T set in the test tube heating / cooling unit 3 shown in FIGS. 4 and 5 are of a general type having a diameter of, for example, 16 mm, and have a length of, for example, 100 mm or 160 mm. The test tube T has a lower end E cut off in, for example, a hemispherical shape, and a lid member FT is attached to the flange FF at the upper end, and in the test tube T, a solvent M as a test object is sealed. Has been. About the quantity of the solvent M accommodated in the test tube T shown in FIG. 5, the height of the liquid level of the solvent M is set so that it may become 5 mm higher than the depth of the hole 11H of the heating part 11, for example. Yes.

  Next, the heat insulating member 12 of the test tube heating / cooling unit 3 shown in FIG. 3 will be described.

  An example of the shape of the heat insulating member 12 is shown in FIG. 4 and is a plate-like member. The heat insulating member 12 is disposed between the cooling box 10 and the heating unit 10. The heat insulating member 12 uses, for example, glass fiber as a main base material, and an inorganic material (borate-based binder, phosphate-based binder, etc.) or an organic material (phenol resin, super heat-resistant epoxy resin, etc.) as a binder ) Is used.

  As shown in FIG. 4, the heat insulating member 12 is a slide plate that can be slid in the Y1 direction or the opposite Y2 direction by slide guide members 18 and 18 arranged on both sides. The sliding operation of the heat insulating member 12 can be performed manually by an operator, for example. Thereby, since the sliding operation of the heat insulation member 12 can be performed without using a drive unit such as a motor, the apparatus can be simplified and miniaturized, and the cost can be reduced.

  As shown in FIG. 4, the heat insulating member 12 has a handle portion 12 </ b> H and a plurality of through holes 19. The number of these through holes 19 is the same as the number of the holding hole portions 13 of the cooling box 10 shown in FIG. 5, and each through hole 19 is a hole through which the corresponding test tube T is passed. The plurality of through holes 19 are arranged in a matrix along the X direction and the Y direction with an interval in the same manner as the holding hole portion 13 of the cooling box 10. The handle portion 12H is a portion for the operator to grip the heat insulating member 12 by hand when sliding the heat insulating member 12 in the Y1 direction and the Y2 direction.

  Moreover, as shown in FIG. 4, the heat insulating member 12 includes a through-hole array region 20 in which five through-holes 19 are arrayed along the X direction, and a blocking region 21 adjacent to the through-hole array region 20. And have. A through hole is not formed in the blocking region portion 21, and the blocking region portion 21 enters between the cooling portion 10 and the heating portion 11 when each test tube T is cooled by the cooling portion 10, and each test This is a portion provided to insulate the tube T and the heating unit 11 from heat.

  FIG. 7A to FIG. 7C show the sliding operation of the heat insulating member 12 of the heat insulating member 12 of the test tube heating and cooling unit 3. The heat insulating member 12 has a through hole array region 20 and a blocking region 21. In addition, since the width in the Y direction of the blocking region 21 is set to be equal to or larger than the diameter of the through hole 19, the following operation can be performed. In FIG. 7A, the heat insulating member 12 is in an initial state that has not yet been slid in the Y2 direction, and the lower end portion E of each test tube T is supported by the blocking region portion 21. In FIG. 7B, after each test tube T rises in the Z2 direction, when the heat insulating member 12 is slid by a predetermined stroke in the Y2 direction, a through hole 19 is provided at a position below the lower end E of each test tube T. Is positioned. In FIG. 7C, the test tubes T are simultaneously lowered in the Z <b> 1 direction, so that each test tube T passes through the through hole 19, and the lower end E of each test tube T is in the hole 11 </ b> H of the heating unit 11. Get in.

  Next, the test tube elevating part 7 shown in FIGS. 1 and 3 will be described.

  The test tube elevating unit 7 shown in FIGS. 1 and 3 includes an elevating handle 22, an elevating platform 23, left and right elevating guide units 24, and an elevating fixing handle 25. As shown in FIG. 7 (A), the test tube elevating / lowering unit 7 elevates and lowers the plurality of test tubes T with respect to the holding hole 13 of the cooling box 10 and the through hole 19 of the heat insulating member 12 so as to be insertable / removable. Used.

  The lifting handle 22 shown in FIG. 3 can be rotated in the R1 direction or the R2 direction around the rotation shaft portion 26 by being grasped by the operator's hand. The elevator 23 can be lowered in the Z1 direction or raised in the Z2 direction along the left and right lifting guide portions 24 as the lifting handle 22 rotates in the R1 or R2 direction. The elevator 23 holds the 25 test tubes T already described so that they can be inserted and removed. The lift fixing handle 25 is provided for maintaining the angle of the lift handle 22 after the lift handle 22 rotates in the R1 direction or the R2 direction.

  Next, a usage example of the test tube reflux apparatus 1 having the above-described configuration will be described.

  As shown in FIG. 3, the lower end E of each test tube T contains a solvent M as a test object in advance. The operator fits the plurality of test tubes T into the hole 23H of the elevator 23 and the corresponding holding hole 13 of the cooling box 10 shown in FIG. The heat insulating member 12 shown in FIG. 3 and FIG. 7A is in an initial state that has not yet been slid in the Y2 direction, and the lower end E of each test tube T is supported on the blocking region portion 21 of the heat insulating member 12. Has been. Thereby, each test tube T is in the state shielded from the heat of the heating unit 11 by the heat insulating member 12.

  When the operator lifts the lifting handle 22 shown in FIG. 3 in the direction R2, as shown in FIGS. 3 to 8, the lifting platform 23 simultaneously lifts the flanges FF of all the test tubes T upward from the heat insulating member 12. Float. At this time, as shown in FIG. 7B, the height V at which the lower end E of the test tube T floats from the heat insulating member 12 is set so that the lower end E of the test tube T does not touch the heat insulating member 12. .

  Subsequently, as shown in FIG. 7B and FIG. 8, the worker holds the handle portion 12H of the heat insulating member 12 and shifts (moves) the heat insulating member 12 in the Y2 direction. As a result, as shown in FIG. 7B, the through hole 19 is positioned immediately below the lower end E of each test tube T, and the lower end E of each test tube T can be inserted into the through hole 19. It becomes a state.

  As shown in FIGS. 8 to 9, when the operator lowers the lifting handle 22 in the R1 direction and lowers the lifting table 23 in the Z1 direction, the lifting table 23 is lowered from the flanges FF of all the test tubes T. Move away from the flange FF. For this reason, as shown in FIG. 9 and FIG. 7C, each test tube T can be freely lowered from the lifting platform 23 and lowered in the Z1 direction, so that the lower end E of each test tube T is insulated at the same time. It passes through the through hole 19 of the member 12 and simultaneously enters the hole 11H of the electric heater of the heating unit 11.

  The solvent M at the lower end E of each test tube T is inserted into the hole 11H of the electric heater of the heating unit 11, and the solvent M is heated (heated) to reflux as shown in FIG. FIG. 12A is a conceptual diagram showing a state in which the solvent in the test tube T is heated and refluxed, and FIG. 12B shows a state in which the solvent in the test tube T is cooled. It is a conceptual diagram.

  As shown in FIG. 10, the operator lifts the lifting handle 22 in the R2 direction after the fixed time elapses after the solvent M is heated (warmed) and the reaction of the solvent M is completed. The lifting platform 23 can lift all the test tubes T in the Z2 direction at the same time by hanging the flange FF of the test tubes T. In this case, the lower end E of each test tube T is separated (floated) from the heat insulating member 12.

  Then, as shown in FIG. 10, when the operator shifts (moves) the heat insulating member 12 in the Y1 direction (frontward direction), as shown in FIG. 7B to FIG. The solvent M in the lower end E of T returns to a state where it is shielded from the heat of the heating part 11 by the intervention of the shielding region part 21. At this time, the position of the lower end E of the test tube T does not touch the heat insulating member 12, and the entire solvent M in the test tube T is positioned at the optimum position in the cooling box 10.

  Next, cooling of the solvent M in each test tube T located in the cooling box 10 is started simultaneously.

  Air B for cooling AR is sent into each air guide part 14 of the cooling box 10 through the air hose branch pipe 4B and the plurality of air hoses 4A from the blower device 6 shown in FIG. As a result, the cooling air AR enters the cooling air supply port 15 from the blowing tip 4C of the air hose 4A, flows in the air guide portions 14 along the Y1 direction, and the solvent M in each test tube T. Can be simultaneously cooled and discharged from the cooling air outlet 16.

  When the cooling of the solvent M in each test tube T is started and a predetermined cooling time elapses, the blower device 6 is stopped, so the cooling (blower) process of the solvent M in each test tube T is stopped. In addition, the cooling time of the solvent M of each test tube T changes with kinds (boiling point) of a solvent. Considering the next step, assuming that the solvent M in the test tube T is cooled to 30 ° C. and the boiling point of the solvent M is 80 ° C., the cooling time is 0.08 ° C./sec. The time is, for example, about 625 sec (about 10 minutes).

  When the cooling of the solvent M in each test tube T is completed in this way, as shown in FIG. 11, the operator lowers the lifting handle 22 in the R1 direction, and the lifting platform 23 is a flange at the upper end of the test tube T. Separate from FF. Thereby, as shown in FIG. 7A, the lower end E of the test tube T is placed on the blocking region portion 21 of the heat insulating member 11. Thereafter, the operator can remove the test tube T from the cooling block 10 and the lifting platform 23.

  However, the diameter of the hole 23H provided in the lifting platform 23 shown in FIG. 7A is slightly larger than the outer diameter of the test tube T so that the test tube T can be easily inserted and removed. The outer diameter of the flange FF at the neck (upper end) of the test tube T is set to be smaller. As a result, the test tube T can be easily inserted into or extracted from the hole portion of the lifting / lowering table 23, and the test tube T can be easily replaced.

  Unlike the case of the embodiment of the present invention, if the operator inserts a plurality of test tubes one by one and is heated in order from the solvent in the set test tube, the solvent in each test tube There will be a difference in the amount of heat given by heating.

  However, in the embodiment of the present invention, a plurality of test tubes T are prepared by inserting them into the lifting platform 23 and the cooling box 10 in advance, and then lowering the plurality of test tubes T to thereby prepare a plurality of test tubes T. The solvent M at the lower end E of the tube T can be brought into contact with the heating unit 11 and heated at the same time. Thereafter, the solvent M at the lower end E of the plurality of test tubes T after heating can be simultaneously cooled by the cooling unit 10. Since the plurality of test tubes T can be raised and lowered at the same time, the solvent M at the lower end portion E of the plurality of test tubes T can be heated uniformly and cooled uniformly. For this reason, even if the amount of the solvent M in the lower end E of the plurality of test tubes T is small, the solvent M in each test tube T can be heated and cooled evenly.

  FIG. 13 (A) shows experimental data of the recovery rate after refluxing for 45 minutes when the solvent M is ethanol water. The height dimension of the aluminum block which is the cooling block 10 in this case is 20 mm.

  The experimental data shown in FIG. 13A is a comparison between “no air cooling” in which cooling air is not supplied to the cooling block 10 and “with air cooling” in which cooling air is supplied to the cooling block 10. Yes. The length of the test tube T is 100 mm and 165 mm. Room temperature is 25 ° C. The temperature of the heating part 11, ie, the temperature of the aluminum block, shows examples of 85 to 90 ° C and 115 to 120 ° C.

  As shown in FIG. 13A, the case of “with air cooling” for supplying cooling air to the cooling block 10 according to the embodiment of the present invention regardless of the temperature of the heating unit 11 is within the scope of the present invention. The recovery rate after the reflux of the solvent M is higher than in the case of “no air cooling” in which the cooling air is not supplied to the cooling block 10 which is another comparative example.

  13B shows the recovery rate when the depth of the heating part (aluminum block) 11 is 20 mm and the recovery rate when the depth is 80 mm, and the temperature of the heating part 11 is 85 to 90 ° C. In this case, the recovery rate is improved as compared with the case of 115 to 120 ° C.

  A maximum recovery rate of 99% is achieved by combining the temperature of the heating unit, supplying cooling air to the cooling block (with forced air cooling), the depth of the heating unit (aluminum block), and the length of the test tube. (0.017 g with one test tube) can be obtained. Thereby, for example, when 200 test tubes are used, it is 3.3 mL in terms of 100% ethanol (specific gravity 0.79).

  The recovery rate is calculated as follows. The calculation method of the recovery rate is container (test tube) weight (a), container weight before heat treatment (a) + solvent weight (b), container weight after heat treatment (a) + solvent weight (b ′) At this time, it can be obtained from the equation 100 × (b′−a) / (b−a).

  FIG. 14A shows a comparative example of the cooling method and shows a temperature change during cooling. The temperature change line L1 of “♦” is temperature data when the test tube T is left inserted in the hole of the electric heater (with heat insulating material) of the heating unit (aluminum block). The temperature change line L2 indicated by “■” is temperature data when the sample is left standing in a suspended state in a test tube stand and naturally cooled after heating.

  Further, the temperature change line L3 indicated by “▲” is the temperature data of the test tube T on the windward side (near the hose outlet) when the air is applied in the same state as “■” after heating. . The temperature change line L4 indicated by “x” is the temperature data of the test tube T downstream (far from the hose outlet) of “▲”.

  The temperature measurement location of each temperature data is the liquid temperature of the solvent in the test tube T (liquid temperature only during cooling). The temperature (environment temperature) is room temperature, which is 25 ° C. this time. As shown in FIG. 14A, the heating temperature is 75.degree. The wind temperature is room temperature and is 25 ° C. The number of test tubes T in the temperature change line L4 indicated by “x” is ten. The distance from the upstream is about 300 mm. The air volume is 20-40 L / min.

  FIG. 14B shows a leaving state as a cooling method of the test tube T in the case of the temperature change line L1 shown in FIG. The electric heater of the heating unit 11 is not energized. FIG. 14C shows a state where only the test tube T in the case of the temperature change line L2 shown in FIG. FIG. 14D shows a state where the test tube T in the case of the temperature change line L3 and the temperature change line L4 shown in FIG.

  As shown in FIG. 14A, the temperature change line L4 and the temperature change line L3 to which the cooling air is applied according to the embodiment of the present invention are the temperature change line L1 and the temperature change line that are not applied with the cooling air as a comparative example Compared to L2, the time for lowering the temperature of the test tube T to about 30 ° C. can be shortened from 1200 seconds to 400 seconds, that is, 1/3.

  The test tube reflux apparatus 1 according to the embodiment of the present invention is a test tube reflux apparatus for heating and refluxing a solvent accommodated in a plurality of test tubes T and then cooling the solvent. The test tube reflux apparatus 1 is disposed on the main body, the main body, a heating unit for heating the solvent in the plurality of test tubes at the same time, an upper part of the heating unit, and passing cooling air. In the cooling unit for simultaneously cooling the solvent in the plurality of heated test tubes, and disposed between the heating unit and the cooling unit to insulate the heat of the heating unit, the solvent in the plurality of test tubes by the heating unit And a heat insulating member having a through hole for passing a plurality of test tubes when heating.

  Thereby, the heating unit can simultaneously heat the solvent in the plurality of test tubes passed through the through holes of the heat insulating member, and the cooling unit is heated in the plurality of heated test tubes while the heat of the heating unit is blocked by the heat insulating member. The solvent can be cooled simultaneously. Therefore, the structure can be simplified and the cost can be reduced, and the test objects in the plurality of test tubes can be simultaneously heated, and then the test objects in the plurality of test tubes can be simultaneously cooled.

  If an operator tries to insert and set a plurality of test tubes one by one, the solvent in the set test tubes will be heated in order, so the amount of heat given by heating to the solvent in each test tube There will be a difference.

  However, in the embodiment of the present invention, the solvent at the lower end of the plurality of test tubes T can be simultaneously heated by being in contact with the heating unit, and then can be simultaneously cooled by the cooling unit. In particular, since the amount of the solvent in the lower ends of the plurality of test tubes T is small, it is necessary that the solvent at the lower ends of the plurality of test tubes T can be heated uniformly and cooled uniformly.

  The heat insulating member has a blocking region portion that blocks between the plurality of test tubes and the heating unit when simultaneously cooling the solvent in the plurality of test tubes by the cooling unit, and the heating unit When the plurality of test tubes are heated by the section, the plurality of test tubes are passed through the through holes of the heat insulating member, and when the plurality of test tubes are cooled by the cooling section, the blocking region portion of the heat insulating member In order to block between the plurality of test tubes and the heating unit, the heat insulating member is slidably disposed between the heating unit and the cooling unit.

  In the test tube reflux apparatus 1, when a plurality of test tubes are heated by the heating unit only by sliding the heat insulating member, the plurality of test tubes are passed through the through holes of the heat insulating member, and the plurality of test tubes are cooled by the cooling unit. In this case, since the plurality of test tubes and the heating unit can be blocked by the blocking region portion of the heat insulating member, the structure can be simplified and the cost can be reduced.

  The width | variety of the interruption | blocking area | region part of a heat insulation member is equivalent or more compared with the diameter of the through-hole of a heat insulation member. Thus, when the test tube is cooled, the insulation region of the heat insulation member can support the test tube, and the heat of the heating unit can be insulated by the insulation region of the insulation member so that it does not reach the cooling part. it can.

  In the test tube reflux apparatus, the arrangement direction of the plurality of test tubes in the cooling unit is deviated from the flow direction of the cooling air passing through the cooling unit. This prevents the cooling air from directly hitting the test tube, reduces the temperature difference between the windward side and the leeward side of the test tube, and prevents the generation of vortex flow of cooling air as much as possible. Airflow loss (resistance) in the cooling section can be reduced.

  In the test tube reflux apparatus, the plurality of test tubes have an elevating unit that ascends and descends so as to be inserted into and extracted from the through hole of the cooling unit and the heat insulating member. Thereby, since a some test tube can be attached or detached simultaneously, the attachment or detachment and exchange operation | work of a some test tube can be performed easily.

  The present invention has been described with reference to the embodiments. However, each embodiment is an example, and the scope of the invention described in the claims can be variously modified without departing from the scope of the invention. .

  For example, in each embodiment of the present invention described above, the slide operation of the heat insulating member 12 shown in FIG. 3 is performed manually by an operator, but automatically using a slide operation device having a motor or the like. You may make it do. The operation of the lifting handle 22 shown in FIG. 3 in the R1 direction and the R2 direction is manually performed by an operator, but is automatically performed using a slide operation device having a motor or the like. May be. The plurality of air hoses 4A having the stretchability of the air supply unit 4 may be, for example, metal air ducts.

DESCRIPTION OF SYMBOLS 1 Test tube recirculation | reflux apparatus 2 Main body part 3 Test tube heating and cooling part 4 Air supply part 5 Operation panel part 6 Blower apparatus 7 Test tube raising / lowering part 10 Cooling box (cooling part)
DESCRIPTION OF SYMBOLS 11 Heating part 12 Heat insulation member 13 Holding hole part 16 of cooling box Air outlet 19 for cooling 19 Through hole 20 of a heat insulation member Through hole arrangement | positioning area | region part 21 of a heat insulation member 22 Barrier area | region part 22 of a heat insulation member Lifting handle 23 Lifting base 23H Elevator hole AR Cooling air M Solvent (test object)

Claims (4)

A test tube reflux apparatus for heating and refluxing a solvent contained in a plurality of test tubes and then cooling the solvent,
The main body,
A heating unit disposed in the main body unit for heating the solvent in the plurality of test tubes at the same time;
A cooling unit that is disposed at the top of the heating unit and that simultaneously cools the solvent in the plurality of heated test tubes by passing cooling air;
A through hole that is disposed between the heating unit and the cooling unit to block the heat of the heating unit and allow the plurality of test tubes to pass when the solvent in the plurality of test tubes is heated by the heating unit. A heat insulation member having
The heat insulating member has a blocking region portion that blocks between the plurality of test tubes and the heating unit when simultaneously cooling the solvent in the plurality of test tubes by the cooling unit,
When the plurality of test tubes are heated by the heating unit, the plurality of test tubes are passed through the through holes of the heat insulating member, and when the plurality of test tubes are cooled by the cooling unit, the blocking of the heat insulating member is performed. to block between the heating unit and the plurality of test tubes by the region unit, the heat insulating member, in between the cooling section and the heating section, characterized by being slidably disposed test tube recirculation system. The width of the cut-off area of the heat insulating member, a test tube recirculation system according to claim 1, characterized that it is equal to or more as compared to the diameter of the through hole of the insulating member. 3. The test tube reflux according to claim 1, wherein an arrangement direction of the plurality of test tubes is deviated from a flow direction of the cooling air passing through the cooling unit in the cooling unit. apparatus. The test tube reflux apparatus according to claim 3 , further comprising an elevating unit that elevates and lowers the plurality of test tubes so as to be inserted into and extracted from the through holes of the cooling unit and the heat insulating member.

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