JP4206168B2 - Fine powder sample filling equipment - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an analytical sample filling apparatus for filling a large number of containers with a fine powder sample used for dating organic compounds contained in shell fossils and sediments.
[0002]
[Prior art]
For example, accelerator mass spectrometry (hereinafter referred to as AMS) is used to measure the age of organic carbon contained in shell fossils and sediments composed of calcium carbonate, for example, by measuring the half-life using carbon-14. Law) is attracting attention in fields such as earth science and archeology. In order to measure by the AMS method, it is necessary to convert solid carbon from carbon dioxide generated by chemically reacting a sample. As a method for producing the carbon, carbon dioxide is reduced using 1 magnesium to obtain amorphous carbon. 2 Carbon dioxide is reacted with metallic lithium to synthesize acetylene and decompose with alternating voltage to form graphite on the aluminum electrode. Carbon dioxide is reduced to graphite with hydrogen using iron as a catalyst. It can be roughly divided into three.
[0003]
Among the three methods described above, the mixing rate of modern carbon in the sample preparation process is low, and three methods are attracting attention as sample preparation methods for measuring carbon-14 measurement in the AMS method. In particular, care should be taken when dealing with a very small amount of sample because contamination with modern carbon is a major problem. Here, in order to reduce carbon dioxide to graphite with hydrogen gas using iron as a catalyst, powdery iron having a purity of 99.9% or more and 325 mesh is used. There are a number of difficulties in filling a carbon sample of this type with a target 2 mmg sample mixed with graphite in a uniform amount in each container.
[0004]
In FIG. 5, a transparent container 3 made of glass, synthetic resin, etc., which is made of a material that is not charged with static electricity and has strength and heat resistance, is housed in a recess 2 provided in the upper center of a portable holder 1. . A long and narrow wire 6 connected to the upper end is suspended from a support rod 5 appropriately held above the holder 1, and the wire 6 has an upper surface opened and has an upright portion around it to accommodate a large amount of sample 8. The through hole 9 provided in the bottom of the body 7 is inserted, and the lower end of the wire 6 is located in the opening 4 provided in the upper part of the container 3.
[0005]
When a minute vibration is transmitted from the outside to the wire 6 through the support rod 5 for a predetermined time, the sample 8 moves downward along the wire 6 inserted through the sample and fills the transparent container 3. In this case, the wire sways from side to side or the fine particles of the sample are blown off due to the influence of air-conditioned air or the like, so that it is difficult to uniformly fill a small number of samples in a large number of containers 3 within a predetermined time. It was.
[0006]
In FIG. 6, an elongated wire 6 having an upper end connected to a support rod 5 appropriately held above a container 3 accommodated in a recess 2 provided in the upper portion of a portable holder 1 is suspended. The inside of the long hole 11 provided in the elongate glass tube 10 which provided the taper-shaped opening part 10a in the upper end is penetrated. The sample 8 is accommodated in the tapered opening 10 a, and the lower end of the wire 6 penetrating through the sample passes through the elongated hole 11.
[0007]
With the lower end of the wire 6 positioned in the opening 4 of the container 3, minute vibrations are transmitted from the outside to the wire 6 through the support rod 5, and the inside of the long hole 11 extends along the wire 6 penetrating through the sample. Is moved downward to fill the container 3 with the sample. In this case, the wire does not sway from side to side or the fine powder sample is not blown off due to the influence of the air-conditioned air. However, if a sample adheres to the inner wall of the glass tube 10 while moving downward in the long glass tube 10, the filling amount becomes insufficient and it is difficult to fill a uniform amount. It was.
[0008]
[Problems to be solved by the invention]
Since the diameter of the container 3 is as thin as about 6 mm and the carbon sample mixed with graphite is fine powder, the inside of the through hole 9 provided in the box 7 or the long hole 11 of the long glass tube is formed into a dumpling shape. It is extremely difficult to uniformly fill a large number of containers with 2 mmg of sample. Further, even if the wire is vibrated from the outside, it is difficult to fill the wire in a uniform amount if the sample adheres to the inner surface of the glass tube or the sample becomes a dumpling and is difficult to fall. In this way, since the sample is as small as 2 mmg, even if about 10% to 0.1-0.2 mmg is reduced, the amount of the sample is insufficient, and an error occurs in the measured value. Had problems.
[0009]
In view of such drawbacks, the present invention accommodates a metal sphere such as platinum, gold, tungsten, etc., which is heavier than iron, which normally closes the dropping hole of the tapered portion, together with the sample in a tapered portion provided in the sample accommodating portion. It is an object to fill a uniform amount while moving a metal sphere up and down by minute vibrations transmitted from the sphere and dropping a sample little by little through a gap formed between the sphere and the drop hole.
[0010]
[Means for Solving the Problems]
According to the first aspect of the present invention, there is provided a housing in which a door can be opened and closed on one side surface, a guide groove is provided in the vertical direction on the other side surface, and at least a front surface portion is formed of a transparent member, and a holder base installed in the housing The movable body is attached to the guide portion established on the other side of the housing so as to be movable up and down, and is attached to the movable body and provided at the tip of the connecting rod passing through the guide groove. A metal that detachably attaches a sample container provided with a small-diameter portion having a small-diameter drop hole connected to the bottom of a tapered portion formed at the lower portion of the container, and closes the drop-hole in the container so as to be opened and closed A holder that contains a spherical body and has a vibration drive source, and a holder on which a sample holder is mounted is located on a straight line passing through the center of the sample holder and below the sample holder. holder The sample container is placed on a table, the movable body is operated to lower the sample container, the small diameter portion of the sample container is inserted into the container, and the vibrating body is vibrated for a predetermined time. The metal sphere accommodated in the taper portion is vibrated to fill the container in a uniform amount from a gap generated between the metal sphere and the drop hole.
[0011]
The holder table according to the invention of claim 2 has a function of blocking vibrations from the outside.
[0012]
The metal sphere according to the invention of claim 3 is platinum heavier than iron.
[0013]
The container according to a fourth aspect of the invention is characterized in that it is formed of a transparent member having a strength and heat resistance made of a material that does not charge static electricity.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of the present invention will be described with reference to the drawings. In FIG. 1, a synthetic resin or a glass plate having at least both side surfaces and a front surface made of a transparent member is formed on the front surface of a sample filling device 13 placed on a desk 12. A substantially rectangular housing 14 is provided. On the right side surface located on one side (right side in FIG. 1) of this sample filling device, there is provided an opening / closing door A that moves in the horizontal direction (perpendicular to the paper surface) and opens and closes.
[0015]
On the desk 12 positioned on the right side of the housing 14, a holder holder 15 having leg pieces at least at both lower portions and having a square planar shape is placed. A large number of mounting holes 16 are provided at regular intervals on the upper surface of the holder holder, and the holders 1 for removably mounting the transparent containers 3 for storing the samples in the mounting holes 16 can be removed. It is placed.
[0016]
A base 18 is provided at the bottom of the housing 14 of the sample filling device 13 in conjunction with the sample filling device, and external vibrations and impacts are not transmitted to the center of the top surface of the base 18. A holder table 19 having a function of blocking is arranged.
[0017]
On the other side of the housing (left side in FIG. 1), that is, in the center portion of the left side surface, a narrow and long guide groove B is provided in the vertical direction. Further, on the other side of the sample filling device 13 (left side in FIG. 1), a guide unit 20 having an appropriate drive source (not shown) is established inside, and the movable body 21 is moved up and down in the guide unit. It is installed as possible.
[0018]
A minute vibration is generated at the tip of the connecting rod 23 that protrudes horizontally on the right side of the movable body 21, that is, on the housing 14 side and is attached through the guide groove B provided on the left side surface of the housing. A vibrating body 26 incorporating a known vibration drive source 25 is attached. A holding hole 28 is provided inside the tip of a holding piece 27 attached in front of the vibrating body 26, and the sample container 30 can be attached to and detached from the holding hole 28 via an elastic ring 29 made of rubber, synthetic resin material, or the like. The elastic ring 29 enhances the adhesion between the sample container 30 and the holding piece 27 to prevent backlash and shaking.
[0019]
2 and 4, the holder is placed on a holder base 19 located on the center upper surface of the base 18 disposed below the vibrating body 26, and is located on a straight line X passing through the center of the sample container 30. The container 3 is accommodated in the recess 2 of the holder 1 placed below the container.
[0020]
As shown in FIG. 4, the sample container 30 is provided with a tapered portion 33 on the inner bottom surface of the accommodating portion 32 having an enlarged diameter portion 31 on the inner surface of the upper end, and a small diameter drop hole 34 connected to the lower end of the tapered portion 33. It has inside and is formed to the lower end of the small diameter part 35. The small diameter portion 35 is formed to have a diameter that can be inserted into the container 3.
[0021]
In the accommodating part 32 of the sample container 30, for example, a sample 8 in which fine powder of graphite and carbon is mixed is accommodated in a large number of containers 3 so as to be sealed in a uniform amount. And in the said accommodating part 32, the metal sphere 36 and the fine powder sample 8 which formed the diameter of the fall hole 34 larger are accommodated so that a movement is possible.
[0022]
Next, the operation of the present embodiment will be described. A holder (not shown) interlocked with the sample filling device 13 is used to hold the holder 1 hooked on the mounting hole 16 of the holder holder 15 placed on the desk 12. While holding and lifting and moving, the door A is opened and inserted into the housing 14 and placed on the holder table 19. Thereafter, the manipulator is moved backward to close the door A. In this case, the holder 1 is located on a straight line X passing through the center of the sample container 30. The interior of the container 3 is empty. Further, since the housing 14 is formed of a transparent member, the researcher can perform the work while directly confirming with the eyes.
[0023]
Next, when the movable body 21 is lowered by operating the drive source for moving up and down in the guide portion 20, the connecting rod 23 moves downward in the guide groove 3, and as shown by a one-dot chain line in FIG. The small-diameter portion 35 of the body enters the container 3 and stops (FIG. 4). Thereafter, the vibration driving source 25 incorporated in the vibrating body 26 is driven to slightly vibrate the sample container 30 attached to the holding piece 27 attached to the vibrating body. Then, the metal sphere 37 accommodated in the taper portion 33 moves up and down by vibration, passes through a gap formed between the raised metal sphere 37 and the upper end of the drop hole 34, and the sample 8 has a small diameter in the small diameter portion 35. A uniform amount is filled into the lower container 3 through the appropriate drop hole 34, and this is repeated.
[0024]
That is, while the vibrating body 26 is vibrated for a certain time, the sample 8 falls through a gap between the metal sphere 37 and the upper end of the drop hole 34. However, when the operation of the vibration driver 25 is stopped after a lapse of a certain time, the drop hole 34 is closed by the metal sphere 37 and the filling of the sample into the container 3 is completed. In this case, since the small-diameter portion 35 provided in the lower part of the sample container 30 has entered the inside of the container 3, even if the small-diameter portion 35 comes into contact with the inner surface of the container 3, the inner wall surface of the container A fine powder sample does not adhere to the inner bottom of the container 3, and for example, a small amount of 2 mmg can be efficiently filled in a short time.
[0025]
When the operation of the vibrating body 26 stops, the movable body 21 rises and returns to the position indicated by the solid line in FIG. Next, the manipulator that opens the door A and enters the housing 14 holds and removes the holder 1 on which the container 3 filled with the sample is mounted, and latches it in the mounting hole 16 of the holder holder 15. The manipulator with the holder 1 removed holds the other holder 1 containing the empty container 3 and repeats the same operation as before to fill the containers with a uniform amount of sample.
[0026]
The sample 8 is filled in the container 3 by vibrating the sample container 30, but the metal sphere 37 is lifted by the minute vibration with the small diameter portion 35 of the sample container entering the container 3, thereby dropping holes. A fine powder sample falls from a gap formed between the sphere and the sphere. Therefore, a fine powder sample that tends to be dumpling-like is crushed into powder when passing through the gap even if it becomes dumpling-like, so that it does not fall inside the dropping hole 34 as a dumpling-like lump. Even if conditioned air acts, the small diameter portion of the sample container is inserted into the container 3 so that it is not affected by the conditioned air, and the vibration of the vibrating body 26 is caused by the door A of the housing 14. Since it is performed in a closed state, it is hardly affected by the flow of conditioned air.
[0027]
Furthermore, since the holder table 19 has a mechanism that is not affected by external vibrations or shocks, it is affected even when a researcher walks in the room or works on the desk. There is no. It should be noted that a mechanism for interrupting impacts and shocks from the outside world is not necessarily required for this apparatus.
[0028]
【The invention's effect】
According to the first aspect of the present invention, the sample container containing the sample and the metal sphere is vibrated in the taper portion connected to the drop hole, so that the fine powder sample is removed from the gap formed between the floating metal sphere and the upper end of the drop hole. In addition, the sample is filled in the container with the small-diameter portion of the sample container inserted into the container, so that the sample does not fall in a dumpling shape and can adhere to the inner surface of the container. Since there is no, it can efficiently fill a uniform amount.
According to the second aspect of the present invention, since the holder table placed on the table part can block vibrations transmitted from the outside, it is possible to effectively and uniformly dispose the fine powder sample without adhering to the inner wall surface of the container. It can be filled one by one.
Since the invention of claim 3 is made of platinum heavier than iron and is not oxidized, it can be used for a long time.
The invention of claim 4 has the advantage that the sample is not attached to the inner wall surface because the container is made of an uncharged material, and since it is transparent, the filled sample can be visually confirmed. .
[Brief description of the drawings]
FIG. 1 shows a form of a sample filling apparatus according to the present invention, and is a partially broken front view.
FIG. 2 is a front view of an enlarged main part in a state in which a holder for holding a container is installed on a holder table below a sample container mounted on a holding piece attached to a vibrating body.
FIG. 3 is a plan view showing a state in which a housing cylinder is attached to a holding piece attached to a vibrating body.
FIG. 4 is an enlarged cross-sectional view of a main part showing a state in which a small diameter portion of a lowered sample container is inserted into a container and filled with a sample.
FIG. 5 is a partially broken explanatory view showing this conventional sample storage device.
FIG. 6 is a partially broken explanatory view showing another conventional sample storage device.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Holder 3 Container 8 Fine powder sample 13 Sample filling apparatus 14 Housing 15 Holder holder 16 Mounting hole 18 Base part 19 Holder base part 20 Guide part 21 Movable body 23 Connection rod 25 Vibration drive source 26 Vibration body 27 Holding part piece 30 Sample Container 33 Tapered part 34 Drop hole 35 Small diameter part 37 Metal sphere
A door
B Guide groove

Claims (4)

A housing in which a door can be opened and closed on one side, a guide groove is provided in the vertical direction on the other side, and at least a front part is formed of a transparent member,
A base portion having a holder base placed in the housing;
A movable body is mounted on the guide portion established on the other side of the housing so as to be movable up and down, and is formed at the tip of a connecting rod that is attached to the movable body and penetrates the guide groove, at a lower portion of a housing portion provided inside. A sample container provided with a small-diameter portion having a small-diameter drop hole connected to the bottom of the tapered portion is detachably attached, and a metal sphere that closes the drop-hole so as to be openable and closable is accommodated and vibrated in the accommodating portion. A holder comprising a vibrating body provided with a driving source and mounted with a holder for accommodating a sample is placed on a straight line passing through the center of the sample container and on the holder table located below the sample container. Then, the movable body is actuated to lower the sample container, the small diameter portion of the sample container is inserted into the container, and the vibrating body is vibrated for a certain period of time to be accommodated in the tapered portion of the sample container. Vibrated metal sphere Fine powder sample filling apparatus, characterized in that to uniform amount at a time filled into the container from the gap formed between the metal spheres with drop hole. 2. The fine powder sample filling apparatus according to claim 1, wherein the holder stage has a function of blocking vibrations from outside. 3. The fine powder sample filling apparatus according to claim 1, wherein the metal sphere is platinum heavier than iron. The fine powder sample filling apparatus according to any one of claims 1 to 3, wherein the container is formed of a transparent member having a strength and heat resistance made of a material that does not charge static electricity.

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