JP5059520B2 - Sample drying equipment - Google Patents

Description

  The present invention relates to a sample drying apparatus for drying a sample for analysis.

  Conventionally, when drying samples for analysis such as powder samples, animal and plant samples, and molded samples obtained by molding powder samples, they are naturally dried, dried using a heater such as an infrared lamp, or dried by a dryer. A drying apparatus provided with a heating and drying means for heating the room and / or a vacuum drying means for evacuating the drying room is used. In the fluorescent X-ray analysis, when a sample solution is analyzed, the sample solution is dropped on a filter paper, and the filter paper is dried by the above-described drying method and apparatus.

  However, in these methods and apparatuses, the sample may be contaminated during drying, and a long time is required for drying. For example, in a conventional vacuum dryer, heating is performed from the side wall, but since the propagation efficiency of heat in vacuum is extremely low, drying takes a long time. In particular, in the fluorescent X-ray analysis in which the sample solution is instilled on the filter paper and the filter paper is dried and measured, the filter paper in which the sample solution is sufficiently soaked takes a long time to dry, and the analysis work can be performed quickly. There wasn't. Moreover, since the trace component (ppm or ppb level) of a solution sample is measured, contamination of a sample is a big problem.

  The present invention has been made in view of the above-described conventional problems, and an object thereof is to provide a sample drying apparatus that dries in a short time without contaminating the sample.

  In order to achieve the above object, a sample drying apparatus of the present invention includes a box-shaped drying chamber in which a sample or a holding body holding a sample is housed and sealed by closing an openable / closable door. A vacuum pump that evacuates the drying chamber; a mounting portion that is provided in the drying chamber and on which a sample or a holding body that holds the sample is mounted; and is directly connected to the lower surface of the mounting portion And a control means for controlling the vacuum pump and the heater.

  According to the sample drying apparatus of the present invention, the drying chamber in which the sample is accommodated is sealed, and a heater such as an infrared lamp is not above the sample, so that the sample is not contaminated. Further, since the drying chamber is evacuated by the vacuum pump, a heater is directly connected to the lower surface of the mounting portion on which the sample or the holding body holding the sample is mounted. Even if it is applied, heat propagation is good, moisture from the sample evaporates quickly, and it can be dried in a short time.

  In the sample drying apparatus of the present invention, the holder holding the sample is a filter paper infused with the sample solution, and the support is placed on the placement unit and supports the peripheral portion of the lower surface of the filter paper. It is preferable to have. Moreover, it is preferable that the holding body holding the sample is a filter paper on which the sample solution is instilled, and a support member that supports the peripheral portion of the lower surface of the filter paper is integrally formed on the mounting portion.

  Since the sample may be contaminated when the lower surface of the filter paper is brought into contact with the mounting portion, it cannot be brought into contact. If these supporting tools are provided or if the supporting tools are formed integrally with the mounting portion, the peripheral portion of the lower surface of the filter paper can be supported while slightly floating the central portion of the lower surface of the filter paper. .

  Hereinafter, the sample dryer 100 which is embodiment of this invention is demonstrated. As shown in FIG. 1, for example, a drying chamber 1 formed in a box shape with a transparent acrylic resin has an openable / closable door 11 through which a sample S to be dried or holders 8 and 9 holding the sample S are taken in and out. It is sealed by closing the door 11. The vacuum pump 2 that evacuates the inside of the drying chamber 1 is, for example, a diaphragm type dry vacuum pump, and the contamination of the sample S is prevented by using the dry vacuum pump.

  The heating table 3 provided at the lower end of the drying chamber 1 has a placement portion 31 on which the sample S or the holding bodies 8 and 9 are placed. As for the mounting part 31, the heater 4 is directly attached to the lower surface 32 thereof. The heater 4 is a sheet-like heater, for example, and is provided on almost the entire lower surface 32. A space under the heater 4 or a part of the heating table 3 may be used. That is, the heater 4 may be incorporated so as to be embedded in the heating table 3. The control means 5 controls the operating time of the vacuum pump 2 and the heating temperature and heating time of the heater 4 according to the set conditions. The control means 5 may individually include a temperature controller of the heater 4, a heating timer, and an operation timer of the vacuum pump 2, or may be configured as a single computer as a whole. The holding body 8 is mounted on a coin-type support 6 described later, and the holding body 9 is mounted on a ring 7 described later.

  3A and 3B includes a peripheral portion 61 projecting upward and a plate-like portion 62. The plate-like portion 62 has a diameter of 28 mm and a thickness of 5 mm, for example, and the peripheral portion 61 protrudes from the upper surface of the plate-like portion 62 by, for example, 0.5 mm. The coin-shaped support 6 is placed on the placement portion 31, contacts the placement portion 31 with the plate-like portion 62, and the first drip which is the holding body 8 at the peripheral portion 61 as shown in FIGS. 5A and 5B. The lower surface 82 of the filter paper 8 is supported. The coin-type support 6 may be any material that has good thermal conductivity and excellent corrosion resistance, and is made of, for example, a metal such as stainless steel or aluminum. In the first drip filter paper 8, a circular PET (polyethylene terephthalate) 83 having a thickness of 1 mm, an outer diameter of 50 mm, and an inner diameter of 40 mm is affixed to the back surface of the mylar film 84, and a circular filter paper 85 having a diameter of 18 mm at the center of the upper surface of the mylar film 84. Is affixed and formed. The sample solution is instilled onto the circular filter paper 85 at the center. The first drip filter paper 8 is used for fluorescent X-ray analysis.

  As shown in FIGS. 5A and 5B, when the first drip filter paper 8 is placed on the coin-shaped support 6, the lower surface of the first drip filter paper is not brought into contact with the placing portion 31 without contacting the lower surface 82 of the first drip filter paper. Since the circular filter paper 85 is close to the coin-type support 6 heated by the heater 4, the radiant heat from the coin-type support 6 is well transmitted. At the same time, since the drying chamber 1 is evacuated by the vacuum pump 2, moisture from the sample S evaporates quickly and can be dried in a short time.

  4A and 4B are ring-shaped supports, for example, a ring 7 having a height of 5 mm, an outer diameter of 35 mm, and an inner diameter of 32 mm. The ring 7 is placed on the placement unit 31, and contacts the upper surface 31 of the heating table 3 at the lower end surface 72 of the ring 7 and supports the lower surface of the second drip filter paper 9 at the upper end surface 71 of the ring 7. The ring 7 may be any material that has good thermal conductivity and excellent corrosion resistance, and is made of a metal such as stainless steel or aluminum. The second drip filter paper 9 is formed by fixing an annular filter paper 94 having an outer diameter of 45 mm and an inner diameter of 21 mm and a 20 mm circular filter paper 95 disposed inside the annular ring with four fixed paraffins 93 and fixing the sample to the circular filter paper 95. The solution is instilled. Since the annular filter paper 94 and the circular filter paper 95 are not connected at a portion other than being fixed by the fixed paraffin 93, the sample solution instilled on the circular filter paper 95 does not diffuse into the annular filter paper 94. The second drip filter paper 9 is also used for fluorescent X-ray analysis.

  As shown in FIGS. 6A and 6B, when the second drip filter paper 9 is placed on the ring 7 and the sample solution is dipped, the lower surface 92 of the second drip filter paper is soaked in the sample solution and tends to hang down. Therefore, the height of the ring 7 is formed higher than the peripheral portion 61 of the coin-type support 6. The periphery of the lower surface 92 of the second drip filter paper can be supported without contacting the filter paper with the heating table 3 due to the height of 5 mm of the ring 7, and the center of the lower surface 92 of the second drip filter paper is the heater 4. Since the drying chamber 1 is evacuated by the vacuum pump 2 at the same time, the moisture from the sample S can be quickly evaporated and dried in a short time.

  Next, the operation of the sample drying apparatus 100 will be described. The control means 5 sets the heating temperature of the heater 4 to, for example, 70 ° C., the heating time to, for example, 20 minutes, and the operating time of the vacuum pump 2 to, for example, 20 minutes. The door 11 (FIG. 1) is opened, and the sample S, the coin-type support 6 and the ring 7 as a ring-type support are placed side by side on the heating table 3 as shown in FIG. As shown in FIG. 5B, the first drip filter paper 8 is placed on the peripheral portion 61 of the coin-type support 6, and the second drip filter paper 9 is placed on the upper end surface 71 of the ring 7 as shown in FIG. 6B. For example, 100 μl of a sample solution is collected with a micropipette (not shown) and dropped on the first drip filter paper 8. Similarly, drip is applied onto the second drip filter paper 9. When the door 11 is closed, the main power source of the sample drying apparatus 100, the power source of the vacuum pump and the heater are turned on, the vacuum valve (not shown) is opened, and the leak valve (not shown) is closed. The filter papers 8 and 9 are heated, and the drying chamber 1 is evacuated by the vacuum pump 2, and drying of the drip filter papers 8 and 9 is started. Due to the operation of the vacuum pump 2, the drying chamber 1 is at a pressure of 0.09 MP (megapascal) (a vacuum referred to in the present invention).

  When the heating time and the operation time of the vacuum pump 2 are finished, the drying time is finished and the drying is finished. The leak valve of the vacuum pump 2 is gradually opened and leaked to return the drying chamber 1 to normal pressure. When the leak is completed, the door 11 is opened, and the sample S and the drip filter papers 8 and 9 are taken out using the tweezers so as not to be contaminated.

  Table 1 shows the drying time of the first drip filter paper 8 and the second drip filter paper 9 when the heating temperature of the heater is set to 70 ° C. As described above, the heating temperature and heating time of the heater 4 and the operation time of the vacuum pump 2 vary depending on the number and amount of the sample S and the drip filter papers 8 and 9 accommodated in the drying chamber 1. Set the heating temperature, heating time and operation time appropriate for the amount to dry. About the 2nd drip filter paper 9, when the heating temperature exceeds 70 degreeC, since the fixed paraffin 93 which has fixed the circular filter paper 95 will melt | dissolve, it is preferable to make it 70 degrees C or less.

  Note that the coin-type support 6 and the ring-type support (ring) 7 may be formed integrally with the placement portion 31. In this case, the heating table is the same as that shown in FIG.

  In the sample drying apparatus 100, since the drying chamber 1 in which the sample S or the holding bodies 8 and 9 holding the sample S are accommodated is sealed and there is no heater such as an infrared lamp above the sample S, the sample S There is no contamination. Further, since the drying chamber 1 is evacuated by the vacuum pump 2, the heater 4 is directly connected to the lower surface 32 of the mounting portion 31 while the sample S or the holding bodies 8 and 9 holding the sample S are dried. Even if the chamber 1 is evacuated, heat propagation is good, moisture from the sample S evaporates quickly, and the chamber 1 can be dried in a short time. When the sample S, which has been required to dry for 2 hours in the conventional method or apparatus, is dried by the sample drying apparatus 100, it takes only 20 minutes. In particular, in the case of a sample having a high sugar content and milk fat content such as milk, the drying time is significantly shortened compared to conventional methods and apparatuses. In addition, since the drying time of the sample is greatly shortened, it is possible to repeatedly perform the operation of instilling the sample solution on the drip filter paper 8 and 9 and drying the sample solution on the drip filter paper 8 and 9 and drying the sample solution. It becomes easy, the sample solution can be concentrated to a higher concentration, and a trace amount of fluorescent X-ray analysis can be performed.

It is a front view of the sample drying apparatus which is embodiment of this invention. It is a top view of the mounting part which has mounted the sample of the apparatus. It is a top view of the coin type support of the device. It is front sectional drawing of the coin-type support tool of the same apparatus. It is a top view of the ring type support tool of the same apparatus. It is front sectional drawing of the ring type support tool of the apparatus. It is the top view which mounted the 1st drip filter paper on the coin type support of the device. It is front sectional drawing which mounted the 1st drip filter paper in the coin-type support tool of the apparatus. It is the top view which mounted the 2nd drip filter paper on the ring type support of the device. It is the front view which mounted the 2nd drip filter paper on the ring type support of the device.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Drying chamber 2 Vacuum pump 3 Heating stand 4 Heater 5 Control means 6 Coin type support tool 7 Ring (ring type support tool)
8 Holder (1st drip filter paper)
9 Holder (2nd drip filter paper)
DESCRIPTION OF SYMBOLS 11 Door 31 Mounting part 32 Lower surface 61 of mounting part Peripheral part 62 Plate-shaped part 100 Sample drying apparatus S Sample

Claims (2)

A filter paper infused with the sample solution is housed inside, and a box-shaped drying chamber sealed by closing the openable door;
A dry vacuum pump for evacuating the drying chamber;
A placement unit provided in the drying chamber, on which the filter paper is placed;
It is mounted on the mounting portion and has a peripheral portion protruding upward to support the peripheral portion of the lower surface of the filter paper, and a plate-shaped portion that contacts the mounting portion, and is formed of a metal having good heat conductivity. A coin-type support tool, or an upper end surface that is placed on the placement portion and supports a peripheral portion of the lower surface of the filter paper, and a lower end surface that contacts the placement portion, and has good heat conduction A ring-shaped support made of metal ;
A heater in which a sheet-like heater is provided on the entire lower surface of the mounting portion;
Control means for controlling the dry vacuum pump and the heater;
A sample drying apparatus. In claim 1,
A sample drying apparatus in which the support is integrally formed on the mounting portion.

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