JPWO2008156114A1 - Powder measuring instrument, sample preparation device, and sample preparation method - Google Patents

Abstract

A housing 81 having a shaft mounting hole 81a and a supply shaft 82 that is rotatably fitted in the shaft mounting hole 81a are provided. A contact surface 82a that contacts an inner peripheral surface of the shaft mounting hole 81a is provided on the outer periphery of the supply shaft 82. And a measuring hole 88 which is surrounded by the contact surface 82a and recedes from the contact surface 82a toward the center in the radial direction, and the housing 81 has the measuring hole 88 of the supply shaft 82 facing upward. A powder introduction hole 86 connected to the measurement hole 88 and a powder extraction hole 87 connected to the measurement hole 88 when the measurement hole 88 is directed downward are provided.

Description

  The present invention relates to a powder measuring device for measuring powder, or a sample preparation apparatus and a sample preparation method for preparing a sample by measuring powder and preparing the powder and a solvent.

  As a device for weighing a certain amount of powder, fill the inside of the through-measuring hole formed in the rod with powder, open the lower part of the through-measuring hole, drop the powder, and weigh a certain amount of powder An apparatus is known (for example, refer to Patent Document 1).

JP 2001-124790 A

  However, the above-described apparatus is not suitable for weighing a very small amount of powder because of its configuration. In addition, the above-mentioned apparatus accurately measures fine powder particles, crystals or crystalline powders having a relatively large particle diameter, and powders that are sticky or that exhibit stickiness when compressed. It is impossible to do. For example, in the case of a fine particle size powder, it has fluidity and may behave like a liquid, so that measurement is difficult. On the other hand, in the case of a crystal or a crystal-like powder having a relatively large particle size, there is a risk of clogging during measurement, and measurement is difficult. In addition, when measuring a powder having adhesiveness or exhibiting adhesiveness at the time of compression, it may be hardened when pressure is applied, and measurement is difficult.

  Therefore, an object of the present invention is to provide a powder measuring instrument and a sample preparation device capable of measuring a small amount of powder.

  The powder measuring instrument of the present invention includes a housing having a shaft mounting hole, and a supply shaft that is rotatably fitted in the shaft mounting hole, and an outer periphery of the supply shaft is provided on an inner periphery of the shaft mounting hole. A contact surface that contacts the surface, and a recess that is surrounded by the contact surface and that recedes from the contact surface toward the center in the radial direction. The recess of the supply shaft is directed upward in the housing. A powder introduction hole that is sometimes connected to the recess and a powder take-out hole that is connected to the recess when the recess of the supply shaft is directed downward are provided. To do.

  According to the powder measuring instrument of the present invention, the powder is stored in the region surrounded by the powder introduction hole and the supply shaft. When the recess appears in the powder introduction hole by the rotation of the supply shaft, the powder is supplied to the recess. Then, the powder that does not fully enter the recess according to the rotation of the supply shaft is slid along the inner peripheral surface of the shaft mounting hole. Thereby, the powder for the area | region enclosed by a recessed part and a shaft attachment hole is hold | maintained at a recessed part. When the recess reaches the powder extraction hole, the powder held by the recess is taken out. Accordingly, a certain amount of powder can be measured by rotating the supply shaft. Since the concave portion is formed so as to be surrounded by the contact surface of the supply shaft, even if the concave portion is formed small, the concave portion is covered with the powder, and the powder can be rubbed through the shaft mounting hole of the housing. Thereby, even a very small amount of powder can be measured.

  In one embodiment of the powder measuring instrument of the present invention, a notch may be provided on a side surface of the powder introduction hole through which the recess of the supply shaft passes. According to this aspect, the notch retains the powder that is about to move according to the rotation of the supply shaft, so that the powder is stored in the notch. Thereby, powder can be reliably supplied to a recessed part.

  In one form of the powder measuring instrument of the present invention, the powder take-out hole is provided with a gas supply port for supplying gas and a nozzle for discharging the powder held in the recess together with the supplied gas. May be. According to this aspect, the gas is blown to the supply shaft by supplying the gas to the powder extraction hole of the housing. The gas blows off the powder held in the recess and is discharged together with the powder from the nozzle. Thereby, all the powders held in the recesses can be taken out.

  One form of the powder measuring instrument of the present invention may further include a vibration motor that applies vibration to the supply shaft. According to this aspect, the powder is pulled away from the supply shaft by applying vibration to the supply shaft. Thereby, powder can be taken out from a recessed part.

  In one form of the powder weighing instrument of the present invention, a plurality of recesses may be provided in the axial direction of the supply shaft. According to this aspect, a plurality of weighings can be performed by one rotation of the supply shaft. Therefore, the time required for weighing can be shortened.

  In the form in which the supply shaft is provided with a plurality of recesses, the plurality of recesses may have different sizes. According to this embodiment, the recesses can be used properly according to the amount of powder required.

  In one form of the powder weighing instrument of the present invention, a plurality of recesses may be provided in the circumferential direction of the supply shaft. According to this embodiment, the powder can be measured a plurality of times at the position of one powder introduction hole while the supply shaft rotates once. Thereby, the time required for weighing can be reduced with a simple configuration.

  In one form of the powder metering instrument of the present invention, a mill part or a function corresponding to it may be further provided for aligning the particle diameter of the powder introduced into the powder introduction hole. According to this form, it is possible to measure without clogging the powder by crushing a crystal or a crystalline powder having a relatively large particle size to make the particle size uniform.

  In one form of the powder measuring instrument of the present invention, a supply pipe that is inserted into the powder take-out hole and opened upward in a state of being rotatable about an axis that is movable in the vertical direction and extends in the vertical direction, A scraping member that is provided at the upper end of the supply pipe and that can be inserted into the recess, and when the recess of the supply shaft is directed downward, the scraping member is rotated in a state of being inserted into the recess. Drive means for driving the supply pipe. According to this aspect, when the recess of the supply shaft is directed downward, the scraping member rotates with the recess inserted, so that the powder sample held in the recess is reliably scraped by the scraping member. Can be led to the supply pipe.

  In this embodiment, the scraping member has a tongue portion that extends in each of the direction of the axis and the direction crossing the recess portion and can be inserted into the recess portion, and the tongue portion has a thickness upward. It may be gradually thinner. In this case, since the surface pressure on the powder sample can be reduced when the tongue is inserted in a state where the powder sample is held in the recess, the powder sample can be prevented from being pressed into the recess. In addition, there is an advantage that the powder sample hardly remains at the tip of the tongue.

  The sample preparation apparatus of the present invention includes the above-described powder weighing instrument, and solves the above-described problems by preparing a sample by blending the powder weighed by the powder weighing instrument and a solvent. According to the sample preparation device of the present invention, powder used for sample preparation can be measured using a powder measuring instrument. A very small amount of powder can be measured, and the labor required for sample preparation can be saved.

  The sample preparation method of the present invention is the above-described problem by measuring powder with the above-mentioned powder measuring instrument, and preparing the sample by mixing the powder measured with the powder measuring instrument and the solvent. To solve. According to the sample preparation method of the present invention, the powder is weighed with a powder measuring instrument, and then the powder and the solvent are mixed to prepare the sample. A very small amount of powder can be measured, and the labor required for sample preparation can be saved.

  As described above, according to the powder measuring instrument of the present invention, when the concave portion appears in the powder introduction hole due to the rotation of the supply shaft, the powder stored in the powder introduction hole is supplied to the concave portion. The powder that does not fit into the recess as the supply shaft rotates is slid along the inner peripheral surface of the shaft mounting hole. Thereby, the powder for the area | region enclosed by a recessed part and a shaft attachment hole is hold | maintained at a recessed part. When the recess reaches the powder extraction hole, the powder held by the recess is taken out. Accordingly, a certain amount of powder can be measured by rotating the supply shaft. Since the concave portion is formed so as to be surrounded by the contact surface of the supply shaft, even if the concave portion is formed small, the concave portion is covered with the powder, and the powder can be rubbed through the shaft mounting hole of the housing. Thereby, even a very small amount of powder can be measured. Moreover, it is possible to accurately measure powders of any nature. For example, even a fine particle size powder having fluidity can be metered in a certain amount, such as a crystal or a crystalline powder having a relatively large particle size, Alternatively, even powders that exhibit tackiness when compressed can be measured without clogging. Moreover, according to the sample preparation apparatus and sample preparation method of the present invention, the powder used for sample preparation can be measured using a powder measuring instrument. A very small amount of powder can be measured, and the labor for sample preparation can be saved.

FIG. 1 is a schematic view of a sample preparation device provided with a powder weighing instrument according to one embodiment of the present invention. FIG. 2 is a detailed view of the powder unit. FIG. 3 is a perspective view illustrating a mill unit, a stirring unit, and a supply unit. FIG. 4 is an enlarged perspective view of the supply unit. FIG. 5A is a diagram illustrating an operation of measuring a powder sample in the supply unit. FIG. 5B is a diagram illustrating an operation following FIG. 5A. FIG. 5C is a diagram illustrating an operation following FIG. 5B. FIG. 6 is a view showing a modified example of the supply shaft. FIG. 7 is a detailed view of the powder unit according to the second embodiment. FIG. 8 is a view showing a cross section taken along line VIII-VIII in FIG. FIG. 9 is an enlarged cross-sectional view of the cross section taken along the line IX-IX in FIG. FIG. 10 is an exploded perspective view illustrating an attachment state of the supply pipe and the scraping member illustrated in FIGS. 7 and 8. FIG. 11 is an explanatory diagram for explaining the operation of the supply pipe shown in FIGS. 7 and 8.

(First form)
FIG. 1 is a schematic view of a sample preparation device provided with a powder weighing instrument according to one embodiment of the present invention. The sample preparation device 1 is a device that automates sample preparation. The sample preparation apparatus 1 includes a powder measuring unit 2 for measuring a powdery sample (hereinafter referred to as a powder sample) as a powder, a powder sample measured by the powder measuring unit 2, a liquid sample, and a solvent. A sample preparation unit 3 for preparing a sample by preparing a sample, a handling unit 4 for holding and moving various containers such as a vial holding a sample and a sample, a screw-capped container, a microplate, and the sample container The access part 5 is provided.

  The powder weighing unit 2 measures a certain amount of powder sample and supplies it to various containers, a scale 12 for weighing various containers, a glove box 13 for isolating the powder unit 11 and the scale 12; , And a monitor 14 for displaying the measurement value on the scale 12. Details of the powder unit 11 will be described later. The scale 12 uses an electronic scale or the like, and measures various containers before and after supplying the powder sample. On the front surface of the glove box 13, gloves for internal work are installed.

  The sample preparation unit 3 includes a capper 21 that opens and closes the lid of the screw lid type container, a decapper 22 that removes the vial capping lid, a capping unit 23 that measures and discards the weight of the removed capping lid, A barcode labeler 24 for attaching barcode labels to various containers, a barcode reader 25 for reading the attached barcode labels, an injection system 26 for injecting liquids and gases into various containers, and alcohol in various containers An alcohol cleaning system 27 for injecting and cleaning, a pump 28 for operating the injection system 26 and the alcohol cleaning system 27, a pH electrode 29 and a pH measuring device 30 for measuring the pH value of the sample or sample, A stirrer 31 to stir the sample and sample, and a pipet to handle the pipette to prepare the sample. And Ttoyunitto 32, a volumetric flask unit 33 for handling a measuring flask to prepare a sample, and various containers, and a preparation device yard 34 for placing an instrument or the like for handling the tablets and capsules. In the sample preparation section 3, the sample is taken out from the container containing the sample, weighed and prepared, and the process up to the preparation of the sample is performed.

  The handling unit 4 moves in the X-axis direction and the Y-axis direction in FIG. 1 and transports various containers. In addition, by attaching an instrument or the like for handling tablets and capsules, things other than various containers can be transported. As such a moving mechanism, for example, a stage unit in which an XY stage and a lifting mechanism are combined can be used.

  The entrance / exit section 5 includes an entrance / exit 41 through which various containers are taken in / out of the sample preparation apparatus 1, and a shuttle 42 that connects the entrance / exit 41 and a position where the handling unit 4 can be moved to reciprocate various containers. Yes. The powder sample weighed by the powder metering unit 2 is mixed with another sample by the sample preparation unit 3 and taken out as a sample prepared from the loading / unloading unit 5.

  FIG. 2 shows a detailed view of the powder unit 11. The powder unit 11 includes a mill unit 51 for uniforming the particle size of the powder sample, an agitation unit 52 for agitating the powder sample averaged by the mill unit 51, and a predetermined amount of the powder sample supplied from the mill unit 51. And a motor 54 for operating the mill unit 51, and a motor 55 for operating the stirring unit 52 and the supply unit 53. An electric motor or the like is used for the motor 54 and the motor 55.

  FIG. 3 is a perspective view showing the mill unit 51, the stirring unit 52, and the supply unit 53. The mill unit 51 includes a mill chamber 61 to which a powder sample is supplied, a mesh 62 installed in the lower part of the mill chamber 61, a fin 63 that rotates in the mill chamber 61a, and a shaft 64 that rotatably supports the fin 63. And a bearing portion 65 that receives the shaft 64, and a miter gear 66 that is fixed to the shaft 64 and receives the driving force from the motor 54. The mill chamber 61a penetrates the mill chamber 61 in the vertical direction. The upper part of the mill chamber 61a is covered with a bearing 65, and a mesh 62 having a mesh diameter suitable for blending is installed at the lower part. The supply of the powder sample to the mill chamber 61 may be performed by providing an auto-feeding device that automatically supplies the powder sample from a container holding the powder sample, or may be performed manually by an operator. Also good. The fin 63 rotates in the mill chamber 61a to crush a crystal sample or a crystalline powder sample having a relatively large particle size, or a powder sample that is fixed or has irregular particle sizes. As a result, the particle size of a crystal or a crystalline powder sample having a relatively large particle size can be made uniform. Then, a powder sample having a particle size equal to or smaller than the mesh diameter of the mesh 62 falls to the stirring unit 52. The stirring unit 52 includes an agitator chamber 71 into which the powder sample from the mill unit 51 is introduced, an agitator 72 that rotates in the agitator chamber 71a to stir the powder sample, and a shaft 73 that rotatably supports the agitator 72. And a gear 74 that is fixed to the shaft 73 and receives a driving force from the motor 55. The lower part of the agitator chamber 71a is hemispherical, and a supply hole 75 is provided at the lower end. The agitator 72 is provided with T-shaped blades 72 a at both ends, and the center thereof is fixed to the shaft 73. As the agitator 72 rotates in the agitator chamber 71a, the powder sample falls from the supply hole 75 while being stirred.

  FIG. 4 shows an enlarged perspective view of the supply unit 53. The supply unit 53 includes a housing 81 having a shaft attachment hole 81a, a supply shaft 82 that is rotatably fitted in the shaft attachment hole 81a, a gear 83 that meshes with the gear 71 and receives the driving force from the motor 55, and argon gas. Are provided with a gas inlet 84 for injecting gas and a nozzle 85 for discharging a powder sample. The housing 81 is provided with a powder introduction hole 86 whose lower end opens into the shaft attachment hole 81a and a powder extraction hole 87 whose upper end opens into the shaft attachment hole 81a. The powder introduction hole 86 is provided at a position corresponding to the supply hole 75 of the stirring unit 52 at the top of the housing 81 and holds the powder supplied from the supply hole 75. The powder extraction hole 87 includes two through holes 87a and 87b that pass between the outside of the housing 81 and the shaft mounting hole 81a, and two through holes when the supply shaft 82 is fitted into the shaft mounting hole 81a. The connecting path 87c is configured such that the inner peripheral surface of the shaft mounting hole 81a moves backward on the radially outer side of the shaft mounting hole 81a so that 87a and 87b are connected.

  On the outer periphery of the supply shaft 82, there are a contact surface 82 a that contacts the inner peripheral surface of the shaft mounting hole 81 a, and a measurement hole 88 that is surrounded by the contact surface 82 a and that is recessed from the contact surface 82 a toward the center in the radial direction. And are provided. The material of the supply shaft 82 is, for example, ceramics or stainless steel. In production of the supply shaft 82, the precision of the shaft and the measuring hole 88 can be increased by polishing. The measurement hole 88 is provided so as to be aligned with the powder introduction hole 86 and the connection path 87 c in the axial direction of the supply shaft 82. Accordingly, when the supply shaft 82 rotates, the measurement hole 88 appears and disappears with respect to the powder introduction hole 86 and the connection path 87c. The measuring hole 88 is formed in a size corresponding to the amount of the powder sample to be measured. The gas supply port 84 and the nozzle 85 are connected to the through holes 87a and 87b, respectively. The argon gas supplied from the gas supply port 84 is blown to the supply shaft 82 and is discharged from the nozzle 85 via the connection path 87c.

  Next, with reference to FIGS. 5A to 5C, an operation for measuring a powder sample in the supply unit 53 will be described. The powder sample stirred by the stirring unit 52 falls from the supply hole 75 and moves to the powder introduction hole 86 of the supply unit 53. When the supply shaft 82 is rotated by driving the motor 55 and the measurement hole 88 appears in the powder introduction hole 86, the powder sample is supplied to the measurement hole 88 as shown in FIG. 5A. The powder introduction hole 86 is provided with a notch 86a (see FIG. 4) on the side surface on the downstream side in the rotation direction of the supply shaft 82 in order to slide the powder sample supplied to the measurement hole 88. The notch 86 a stores a powder sample that moves and stays in the rotation direction of the supply shaft 82. Thereby, a powder sample can be reliably supplied to the measurement hole 88.

  Then, as shown in FIG. 5B, the measurement hole 88 passes through the notch 86 a by the rotation of the supply shaft 82. At this time, the notch 87 a slides the powder sample along the contact surface 82 a of the supply shaft 82. Therefore, the powder sample held by the measuring hole 88 becomes a certain amount. When the supply shaft 82 further rotates and the measuring hole 88 reaches the lower side as shown in FIG. 5C, argon gas is supplied from the gas supply port 84. Argon gas is blown to the supply shaft 82, passes through the connecting path 87c, and blows off the powder sample held in the measuring hole 88. The powder sample is discharged from the nozzle 85 together with argon gas. If the tip of the nozzle 85 is inserted into various containers, a certain amount of powder sample is supplied to the various containers. By repeating the above operation, a certain amount of powder sample can be supplied to each of the plurality of containers.

  In the first embodiment, argon gas is supplied from the gas supply port. However, the present invention is not limited to this, and a gas according to conditions may be used. For example, an inert gas such as nitrogen or air may be used. Moreover, in the mill part 51, although the particle size was equalized by crushing a powder sample by rotation of the fin 63, it is not restricted to this, You may utilize various well-known crushing techniques, such as a ball mill.

  In the first embodiment, the example in which one measuring hole 88 is provided in the supply shaft 82 has been described. However, the present invention is not limited to this. A plurality of measuring holes may be provided in the supply shaft 82. For example, as shown in FIG. 6, measuring holes 88 a, 88 b, 88 c having different sizes may be provided continuously in the longitudinal direction of the supply shaft 82. The measuring holes 88a, 88b, 88c may be provided with measuring holes 88d, 88e, 88f in a rotational direction. You may provide a measurement hole for every predetermined angle, for example, every 90 degree | times. The upper surface of the housing 81 may be provided with powder introduction holes corresponding to the positions of the measurement holes 88a, 88b, and 88c. Alternatively, the powder introduction holes may be integrally formed to correspond to the measurement holes. Each notch may be provided. You may form a powder introduction hole, without providing a notch. Even in this case, the powder sample can be rubbed on the side surface of the powder introduction hole. What is necessary is just to comprise the supply hole 75 of the stirring part 52 according to the shape of a powder introduction hole. The nozzles may be provided according to the number of measuring holes that are continuous in the longitudinal direction. What is necessary is just to arrange | position the powder extraction hole 87 so that the powder sample measured by each measurement hole may not mix. Depending on the amount of powder sample desired, the passages may be changed so as to be merged. In this case, the amount of the powder sample weighed in each measuring hole can be combined and discharged from one nozzle, and the degree of freedom of weighing can be increased.

  In the first embodiment, the powder sample held in the measuring hole 88 has been described as an example in which the powder sample is discharged from the nozzle 85 by blowing it off with argon gas, but the present invention is not limited to this. For example, the supply shaft 82 may be vibrated by attaching a vibration motor to the opposite end of the supply shaft 82 of the supply portion 53 to the gear 83. By driving the vibration motor when the measuring hole 88 is positioned on the lower side, the powder sample held in the measuring hole 88 falls. The nozzle may also be vibrated. The mobility of the powder sample is improved. The powder introduction hole 86 and the powder extraction hole 87 are not limited to the example in which the positions are aligned in the axial direction of the supply shaft 82, and the powder introduction hole 86 and the powder extraction hole 87 are connected to the axis. The position in the direction may be shifted. In this case, a drive mechanism capable of reciprocating the supply shaft 82 in the axial direction may be provided, and the supply shaft 82 may be moved in the axial direction while rotating the supply shaft.

(Second form)
Next, a second embodiment of the present invention will be described with reference to FIGS. FIG. 7 is a detailed view of the powder unit 91 according to the second embodiment, and FIG. 8 shows a cross section taken along line VIII-VIII of FIG. The powder unit 91 shown in these drawings can be used by being incorporated in the sample preparation apparatus 1 of FIG. 1 in place of the powder unit 11 of the first embodiment.

  The powder unit 91 includes an agitation unit 92 for agitating the powder sample, and a supply unit 93 as a powder metering instrument that measures the powder sample agitated by the agitation unit 92 by a fixed amount and supplies the powder sample to various containers. Yes. Note that a cap (not shown) may be put on the opening at the top of the stirring unit 92. In addition, the mill unit 51 according to the first embodiment is attached to the upper part of the stirring unit 92, and a crystal or a crystal-like powder sample having a relatively large particle size is crushed by the mill unit 51 to obtain a uniform particle size. A powder sample having a uniform diameter can also be supplied to the stirring unit 92. Furthermore, it is also possible to attach a container such as a commercially available bottle containing a powder sample to be weighed upside down so that its mouth portion faces downward, and is attached to the upper portion of the stirring unit 92. The attachment can be realized, for example, by forming a female screw portion that meshes with a male screw portion formed in the mouth portion of the container on the upper inner peripheral surface of the stirring portion 92 and screwing the mouth portion into the stirring portion 92.

  The agitator 92 is an agitator chamber 94 for agitating the powder sample, an agitator 95 that rotates in the agitator chamber 94a to agitate the powder sample, a shaft 96 that rotatably supports the agitator 95, and a shaft 96 fixed to the agitator 96. And a gear 98 that receives the driving force from the motor 97. The gear 98 meshes with a motor gear 99 fixed to the motor shaft 97a of the motor 97. As the motor 97, a DC electric motor is used. The lower part of the agitator chamber 94a is formed in a semi-cylindrical shape, and a supply hole 100 is provided at the lower end thereof. The agitator 95 is provided with T-shaped blades 95 a at both ends, and the center thereof is fixed to the shaft 96. As the agitator 95 rotates in the agitator chamber 95a, the powder sample falls from the supply hole 100 while being stirred.

  The supply unit 93 includes a housing 101 having a shaft attachment hole 101a and a supply shaft 102 that is rotatably fitted in the shaft attachment hole 101a. The supply shaft 102 has a large-diameter portion 103 fitted in the shaft mounting hole 101a, and a support portion 104 that is coaxial with the large-diameter portion 103 and has an outer diameter smaller than that of the large-diameter portion 103, and these rotate together. It is configured by being combined in a possible state. The material of the large diameter portion 103 is, for example, ceramics, and the material of the support portion 104 is, for example, stainless steel. Between the large-diameter portion 103 and the support portion 104, a rotation preventing means such as a pin for preventing the relative rotation is interposed. The support portion 104 is rotatably provided on the housing 102 via a bearing 105. A gear 106 is fixed to the end portion of the support portion 104. The gear 106 meshes with a motor gear 108 fixed to the motor shaft 107 a of the motor 107. As the motor 107, a pulse motor that can be easily synchronized with a motor 125 described later is used.

  The housing 101 is provided with a powder introduction hole 110 common to the supply hole 100 of the stirring unit 92 whose lower end opens into the shaft attachment hole 101a, and a powder extraction hole 111 whose upper end opens into the shaft attachment hole 101a. It has been. The powder introduction hole 110 holds the powder supplied from the stirring unit 92.

  On the outer periphery of the supply shaft 102, there are a contact surface 102 a that contacts the inner peripheral surface of the shaft mounting hole 101 a, and a measuring hole 112 that is surrounded by the contact surface 102 a and that is recessed from the contact surface 102 a toward the center in the radial direction. And are provided. The measurement hole 112 is formed in a substantially circular shape, and is provided so as to be aligned with each of the powder introduction hole 110 and the powder extraction hole 111 in the axial direction of the supply shaft 102. Thus, when the supply shaft 102 rotates, the measurement hole 112 appears and disappears with respect to the powder introduction hole 110 and the powder extraction hole 111. The measuring hole 112 is formed in a size corresponding to the amount of the powder sample to be measured.

  In the second embodiment, by rotating the supply shaft 102 and sliding the powder sample that does not fit into the measuring hole 112 with the inner peripheral surface of the shaft mounting hole 101a, the supply unit 93 can put a certain amount of powder into the measuring hole 112. The operation until taking the body sample is the same as in the first embodiment (see FIGS. 5A and 5B). The second mode is characterized in that a certain amount of powder sample taken into the measuring hole 112 can be reliably taken out from the measuring hole 112.

  In order to reliably take out a certain amount of powder sample taken into the measurement hole 112, the supply section 93 is provided with a powder take-out mechanism 115. The powder take-out mechanism 115 includes a supply pipe 116 inserted into the powder take-out hole 111, a scraping member 117 provided at the upper end portion 116 a of the supply pipe 116, and a drive mechanism 118 as drive means for driving the supply pipe 116. And.

  The supply pipe 116 opens upward and downward, and an upper end portion 116a has an outer diameter larger than that of other portions. The supply pipe 116 is inserted into the powder extraction hole 111 so as to be movable in the vertical direction and rotatable about the axis Ax extending in the vertical direction.

  9 is an enlarged cross-sectional view of the cross section taken along the line IX-IX in FIG. 8, and FIG. 10 is an exploded perspective view for explaining the attachment state of the supply pipe 116 and the scraping member 117. As shown in detail in FIGS. 9 and 10, the scraping member 117 includes a tongue portion 119 extending in the direction of the axis Ax and a direction crossing the measuring hole 112, and a support portion that supports the proximal end of the tongue portion 119. 120. As shown in FIG. 10, the scraping member 117 has a support portion 120 fitted in a mounting groove 121 formed in the tip end portion 116 a of the supply pipe 116, and is fixed so as not to be easily detached from the supply pipe 116. Yes. The width of the tongue 119 is smaller than the inner diameter of the measuring hole 112 so that the tongue 119 can be inserted into the measuring hole 112 (see FIG. 9). Further, the thickness of the tongue 119 is gradually reduced upward. For this reason, when the tongue portion 119 is inserted in a state where the powder sample is held in the measurement hole 112, the surface pressure on the powder sample can be reduced, so that the powder sample is prevented from being pressed into the measurement hole 112. it can. In addition, there is an advantage that the powder sample hardly remains on the upper end of the tongue 119.

  The drive mechanism 118 shown in FIGS. 7 and 8 rotates so that the tongue 119 of the scraping member 117 is inserted into the measuring hole 112 when the measuring hole 112 of the supply shaft 102 is directed downward. This is a device for driving the supply pipe 116. In order to realize such a function, the drive mechanism 118 moves in the direction of the axis Ax while rotating the supply pipe 116 and the motor 125 that is a drive source, the transmission unit 126 that transmits the rotation of the motor 125 to the supply pipe 116. Conversion section 127 for the above. A pulse motor is used as the motor 125 in order to easily synchronize with the motor 107 on the supply shaft 102 side.

  The transmission unit 126 includes a motor gear 128 fixed to the motor shaft 125a, and a driven gear 129 that meshes with the motor gear 128 and rotates integrally with the supply pipe 116. The driven gear 129 is attached to a positioning collar 130 fixed to the supply pipe 116 via fastening means (not shown) such as a set screw.

  The conversion unit 127 includes a cylindrical male screw member 130 disposed on the outer periphery of the supply pipe 116 and fixed to the driven gear 129, and a female screw 131a that meshes with the male screw 130a formed on the outer periphery of the male screw member 130 on the inner periphery. The female screw member 131 is provided. The female screw member 131 is fixed to the housing 101, and a part of the male screw member 130 is screwed into the female screw member 131 by a predetermined amount. The screws 130a and 131a meshing with each other are configured as trapezoidal screws, and their pitches are set as appropriate.

  With the above configuration, by rotating the motor 125 of the drive mechanism 118, the supply pipe 116 and the scraping member 117 attached thereto can be moved in the vertical direction while rotating around the axis Ax.

  The operation of the motor 125 is controlled together with the motor 107 on the supply shaft 102 side by a computer (not shown). Hereinafter, an example of motor control performed by the computer will be described. FIG. 11 is an explanatory diagram for explaining the operation of the supply pipe 116. 7 and 8, first, the motor 107 is controlled so that the rotation of the supply shaft 102 is temporarily stopped when the supply shaft 102 is directed downward. Then, while the rotation of the supply shaft 102 is temporarily stopped, the scraping member 117 is inserted into the measuring hole 112 of the supply shaft 102 from the position (origin position) in FIG. 8 where the scraping member 117 does not interfere with the supply shaft 102. The motor 125 is controlled so that the supply pipe 116 moves upward while rotating to the inserted position of FIG. As a result, the scraping member 117 rotates while being inserted into the measuring hole 112, so that the powder sample held in the measuring hole 112 is reliably scraped and supplied by the scraping member 117 (tongue 119). Guided to tube 116. Thereafter, the motor 125 is reversely rotated to return to the origin position in FIG. The origin position is detected by the photo sensor 133 (FIG. 7). The amount of movement of the supply pipe 116 is controlled by managing the number of pulses supplied to the motor 125 from the signal from the photosensor 133 as a starting point.

  Also in the second embodiment described above, it can be appropriately changed as in the first embodiment. For example, a plurality of measuring holes may be provided on the supply shaft 102 of the second form as shown in FIG. Further, the supply shaft 102 can be changed to one having a uniform shaft diameter.

  In addition, in either the first form or the second form, when a plurality of measuring holes of different sizes are provided in the supply shaft in the longitudinal direction as shown in FIG. 6, the supply shaft is arranged in the axial direction. A drive mechanism (not shown) that can be moved can be provided. This drive mechanism moves the supply shaft in the axial direction to change the correspondence between the plurality of measurement holes and the single powder extraction hole, so that a powder sample can be obtained using a single powder measurement instrument. It becomes possible to weigh into different quantities.

  The constituent elements such as the mill unit, the stirring unit, and the supply unit of the powder unit according to each embodiment may be made of any material. For example, if a resin material such as polycarbonate is selected as the material of these constituent elements, it can be manufactured at a low cost because the processing effort and material cost can be reduced as compared with the case of using a metal material. Therefore, the powder unit can be made disposable by constituting these constituent elements with resin materials. Further, by constituting these constituent elements with a transparent resin material, it is possible to observe the measuring process of the powder sample from the outside. Thereby, it is possible to quickly find out the malfunction of the powder unit and its cause.

Claims (12)

A housing having a shaft mounting hole;
A supply shaft rotatably fitted in the shaft mounting hole,
The outer periphery of the supply shaft is provided with a contact surface that comes into contact with the inner peripheral surface of the shaft mounting hole, and a recess that is surrounded by the contact surface and that recedes from the contact surface toward the radial center.
The housing has a powder introduction hole connected to the recess when the recess of the supply shaft is directed upward, and a powder connected to the recess when the recess of the supply shaft is directed downward. A powder measuring instrument provided with a body extraction hole.   The powder measuring instrument according to claim 1, wherein a notch is provided on a side surface of the powder introduction hole through which a concave portion of the supply shaft passes.   The powder metering according to claim 1 or 2, wherein a gas supply port for supplying a gas and a nozzle for discharging the powder held in the recess together with the supplied gas are attached to the powder extraction hole. Instruments.   The powder measuring instrument according to any one of claims 1 to 3, further comprising a vibration motor that applies vibration to the supply shaft.   The powder measuring instrument as described in any one of Claims 1-4 which provided the some recessed part in the axial direction of the said supply shaft.   The powder weighing instrument according to claim 5, wherein the plurality of recesses have different sizes.   The powder measuring instrument according to any one of claims 1 to 6, wherein a plurality of recesses are provided in a circumferential direction of the supply shaft.   The powder measuring instrument according to any one of claims 1 to 7, further comprising a mill part or a function corresponding to the same to adjust the particle diameter of the powder introduced into the powder introduction hole.   A supply pipe that is inserted into the powder take-out hole so as to be movable in the vertical direction and that can rotate about an axis extending in the vertical direction, and that opens upward, and is provided at the upper end of the supply pipe. An insertable scraping member; and a driving means for driving the supply pipe so that the scraping member rotates with the recess inserted into the recess when the recess of the supply shaft is directed downward. The powder measuring instrument according to claim 1, further comprising:   The scraping member has a tongue that extends in each of the direction of the axis and in a direction crossing the recess, and can be inserted into the recess, and the thickness of the tongue gradually decreases upward. The powder measuring instrument according to claim 9.   A sample preparation device comprising the powder weighing instrument according to any one of claims 1 to 10, and preparing a sample by blending the powder weighed by the powder weighing instrument and a solvent.   A method for preparing a sample, comprising: measuring a powder with the powder measuring instrument according to any one of claims 1 to 10; and preparing a sample by mixing the powder measured with the powder measuring instrument and a solvent.

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