Sample destruction device, sample destruction unit, and analytical method

Abstract

This facilitates the cleaning and positioning of the tip (tip) of the destructive tool. It also facilitates the handling of samples. [Solution] A sample destruction unit 20 is placed inside the destruction chamber. The sample destruction unit 20 has a main body 64 and a guide 60, as well as a tip 56. The main body 64 has a bottom surface 90 on which the sample 54 is placed. The sample 54 on the bottom surface 90 is covered with a mesh sheet 94. Motive force from the shaft 24 is applied to the tip 56, and the tip 56 destroys the sample 54. The gas released from inside the sample 54 due to the destruction is analyzed.

Description

[[Technical Field]]

[0001] The present invention relates to a sample breaking apparatus, a sample breaking unit, and an analysis method, and particularly relates to a technique for breaking a sample to extract gas from inside the sample. [[Background Art]]

[0002] A sample breaking apparatus is an apparatus that breaks a sample to extract gas from inside the sample for the purpose of inspecting, evaluating, etc. the sample. A sample breaking apparatus can also be referred to as a sample crushing apparatus or a gas extraction apparatus.

[0003] The gas extracted by the sample breaking apparatus includes gas sealed inside the sample during the sample production process, gas that unnecessarily entered the sample during the sample production process, gas generated inside the sample after sample production, and the like. The extracted gas is analyzed. For example, the extracted gas is sent to a mass spectrometer.

[0004] Various samples can be cited as samples to be broken. Such a sample is, for example, an electronic device. A specific example thereof is a crystal oscillator. In recent years, extremely small crystal oscillators have been put into practical use. It is not easy to extract an extremely small amount of gas from such a sample for analysis.

[0005] Patent Document 1, Patent Document 2, and Patent Document 3 each disclose a sample breaking apparatus. The sample breaking apparatus includes a breaking tool for breaking a sample. The breaking tool has a tip end, and the sample is broken (crushed, cut, etc.) by the tip end. Conventionally, the breaking tool is configured as a single member as a whole, that is, only the tip end of the breaking tool cannot be removed. Patent Document 1, Patent Document 2, and Patent Document 3 do not disclose a carrier for holding and transporting a sample or the like. [[Prior Art Documents]] [[Patent Documents]]

[0006] [[Patent Document 1]] Japanese Unexamined Patent Publication No. 2017-58241 [Patent Document 2] Japanese Patent Publication No. 2016-80679 [Patent Document 3] Japanese Patent Application Publication No. 07-288098 [Overview of the project] [Problems that the invention aims to solve]

[0007] Conventional sample destruction devices have several problems, which are described below.

[0008] After sample destruction, the tip of the destruction tool needs to be cleaned. Conventionally, the destruction tool is attached to the housing of the sample destruction device, and it is not easy to remove the destruction tool from the housing. The destruction chamber inside the housing is generally a small space. Cleaning the tip of the destruction tool inside the destruction chamber is also difficult. In conventional destruction devices, if the tip of the destruction tool wears out, the entire destruction tool must be replaced. Such work is troublesome.

[0009] It is desirable to select the tip shape of the destructive tool according to the type and size of the sample. For example, for extremely small and hard devices, it is desirable to use a destructive tool with a hammer-like tip. For devices of a certain size, it is desirable to use a destructive tool with a blade or needle-like tip. It is cumbersome to change the entire destructive tool depending on the type and size of the sample.

[0010] Precise alignment of the central axis of the destructive tool with the sample is required, but such alignment is not always easy due to assembly errors, etc. A mechanism that allows the central axis of the tip to naturally align with the center of the sample is desirable.

[0011] When destroying extremely small samples, vibrations and air currents can easily cause the sample to move on the sample mounting surface before destruction. The sample may also fall off the mounting surface. Sample loss is also likely during transport to the destruction chamber.

[0012] The object of the present invention is to solve at least one of the above-mentioned problems. The object of the present invention is to enable easy cleaning of the tip of a destructive tool (hereinafter also referred to as the tip). Alternatively, the object of the present invention is to enable easy replacement of worn parts of a destructive tool. Alternatively, the object of the present invention is to enable easy selection of the tip shape of a destructive tool. Alternatively, the object of the present invention is to enable accurate positioning of the tip of a destructive tool relative to a sample. Alternatively, the object of the present invention is to enable proper handling of a sample before sample destruction. [Means for solving the problem]

[0013] The sample destruction apparatus according to the present invention comprises a housing having a destruction chamber, and a destruction tool that destroys the sample in the destruction chamber in order to extract gas from inside the sample, wherein the destruction tool comprises a shaft that is movably held by the housing, and a tip that is a member separate from the shaft and destroys the sample by the kinetic force transmitted from the shaft.

[0014] The sample destruction unit according to the present invention is a sample destruction unit that is disposed in the destruction chamber of a sample destruction device that extracts gas from inside a sample, and is a member separate from the shaft provided in the sample destruction device, and includes a tip that destroys the sample by the kinetic force transmitted from the shaft, and a holder that has a sample stage on which the sample is placed, holds the tip and guides the movement of the tip, wherein the sample is placed between the sample stage and the tip before the sample is destroyed.

[0015] The analytical method according to the present invention is characterized by comprising the steps of: placing a sample on a sample stage in a holder; arranging a chip for destroying the sample on the holder, thereby creating a state in which the sample is sandwiched between the sample stage and the chip; arranging a sample destruction unit having the holder and the chip in the destruction chamber of a sample destruction device; transmitting kinetic force from a shaft provided in the sample destruction device to the chip to destroy the sample with the chip, thereby extracting gas from the sample; analyzing the gas extracted from the sample; and removing the sample destruction unit from the destruction chamber after the gas has been extracted from the sample.

[0016] The sample destruction apparatus according to the present invention includes a housing having a destruction chamber, a destruction tool for destroying the sample in the destruction chamber in order to extract gas from inside the sample, and a holder for holding the sample, wherein the destruction tool has a tip for destroying the sample, and the holder has a guide for guiding the tip toward the sample. [Effects of the Invention]

[0017] According to the present invention, the tip of the destructive tool can be easily cleaned. Alternatively, according to the present invention, worn parts of the destructive tool can be easily replaced. Alternatively, according to the present invention, the tip shape of the destructive tool can be easily selected. Alternatively, according to the present invention, the tip of the destructive tool can be accurately positioned relative to the sample. Alternatively, according to the present invention, the sample can be handled appropriately before being destroyed. [Brief explanation of the drawing]

[0018] [Figure 1] This figure shows a gas analysis system according to an embodiment. [Figure 2] This is an xz cross-sectional view of the sample destruction device according to the embodiment. [Figure 3] This is a cross-sectional view of the sample destruction device according to the embodiment, using the yz direction. [Figure 4] This is a diagram showing a conveying device. [Figure 5] It is an xz cross-sectional view of the sample breaking unit according to the embodiment. [Figure 6] It is a yz cross-sectional view of the sample breaking unit according to the embodiment. [Figure 7] It is an exploded perspective view of the sample breaking unit according to the embodiment. [Figure 8] It is a perspective view of the sample breaking unit according to the embodiment. [Figure 9] It is a diagram illustrating the action of a pair of magnets. [Figure 10] It is a diagram showing the chip set. [Figure 11] It is a flowchart showing the analysis method according to the embodiment. [Figure 12] It is a diagram showing a modified example of the sample breaking unit. [Figure 13] It is a diagram showing a first example of the unit replacement mechanism. [Figure 14] It is a diagram showing a second example of the unit replacement mechanism. [Figure 15] It is a diagram showing a modified example of the gas analysis system. DETAILED DESCRIPTION OF EMBODIMENTS

[0019] Hereinafter, embodiments will be described with reference to the drawings.

[0020] (1) Summary of the embodiment (1-1) The sample breaking apparatus according to the embodiment includes a housing and a breaking tool. The housing has a breaking chamber. The breaking tool is a member that breaks a sample in the breaking chamber to extract gas from the interior of the sample. The breaking tool is composed of a shaft and a tip. The shaft is movably held by the housing. The tip is a member separate from the shaft, and breaks the sample by the kinetic force transmitted from the shaft.

[0021] In the above configuration, the shaft and tip are separate components; that is, the tip is separated or independent from the shaft. Therefore, for example, the tip can be easily cleaned outside the destructive chamber. Alternatively, if the tip is worn, it can be easily replaced with a new one. Or, if necessary, it is possible to select a tip with a desired shape.

[0022] In embodiments, the shaft is held directly or indirectly by the housing. For example, the shaft is movably held by a retaining member provided in the housing. The shaft may be driven by the user or by an actuator. Various forms of shafts can be used. The tip may be called a breaking tip, breaking pin, or breaking probe. In embodiments, the breaking chamber is an airtight space. In this specification, the meaning of breaking may include crushing, cutting, drilling, etc.

[0023] In this embodiment, the shaft has a drive end. The tip has a receiving end that receives a kinetic force from the drive end and an acting end that applies the kinetic force to the sample to destroy it. In this embodiment, the drive end has a flat pressing surface, and the receiving end has a flat receiving surface. The pressing surface and the receiving surface are joined together, and a kinetic force is applied from the pressing surface to the receiving surface. A first engagement structure may be provided on the drive end, and a second engagement structure may be provided on the receiving surface. In the engaged state of the first and second engagement structures, a kinetic force may be transmitted from the shaft to the tip.

[0024] The sample destruction device according to this embodiment includes a plurality of tips, each having a different working end. The tip used to destroy the sample is selected from among the plurality of tips. With this configuration, an appropriate tip can be selected according to the hardness, size, etc., of the sample.

[0025] The sample destruction apparatus according to this embodiment includes a holder that holds both the sample and the chip. The holder and the chip constitute a sample destruction unit. The sample destruction unit is placed in the destruction chamber before sample destruction and removed from the destruction chamber after sample destruction.

[0026] The sample destruction unit is a portable unit that functions as both a sample holder and a tip holder. The sample destruction unit ensures accurate positioning of the tip relative to the sample, even if the shaft has assembly errors. Furthermore, the sample destruction unit facilitates the transport of the sample to the destruction chamber before destruction and facilitates the removal of multiple fragments from the destruction chamber after destruction. The sample destruction unit is transported by the user or by an automated transport mechanism.

[0027] In one embodiment, the holder includes a body having a cavity and a guide positioned within the cavity to guide the movement of the tip. The body includes a sample stage facing the cavity. The sample is held between the sample stage and the tip before sample destruction.

[0028] With the above configuration, the free movement of the sample can be restricted before sample destruction, preventing problems such as sample detachment or loss. Since the main body and guide are separate components, the guide can be removed from the main body. With the guide removed, access to the sample stage becomes easier. In other words, the work efficiency when cleaning the sample stage can be improved.

[0029] Multiple fragments generated by the destruction of the sample remain within the sample destruction unit. Removing the sample destruction unit from the destruction chamber removes the contaminated tip and multiple fragments. Typically, the tip, sample stage, etc., are cleaned outside the destruction chamber.

[0030] In one embodiment, the guide has a channel through which gas released from the sample upon disruption of the sample flows. This configuration allows the gas to be transferred to the analyzer without significant diffusion. The shape of the cavity and the tip are determined so as to minimize the volume of the space between the sample and the inlet of the channel.

[0031] In this embodiment, the sample stage is a recess having a bottom surface on which the sample is placed. The guide has an annular lower end that is inserted into the recess. The sample on the bottom surface is covered with a mesh sheet. The annular lower end presses against the mesh sheet around the sample. The protrusion, which will be described later, corresponds to the annular lower end.

[0032] Before sample fracture, the mesh sheet deforms at its annular lower end, thereby holding the sample in place and restricting its movement. After sample fracture, the mesh sheet traps the multiple fragments generated by the fracture, preventing them from scattering.

[0033] The sample breaking device according to the embodiment includes a magnet that generates a magnetic field that exerts a magnetic force on at least one of the sample and the chip. In the embodiment, the magnet is located below the sample stage in the sample breaking unit. A single magnet or multiple magnets may be arranged.

[0034] In one embodiment, the sample is magnetic. In this case, the movement of the sample on the sample stage in the holder is restricted by magnetic force. In another embodiment, the sample has magnetic anisotropy. In this case, the position and orientation of the sample on the sample stage are determined by magnetic force. In yet another embodiment, the tip is magnetic. In this case, a pressing force is applied from the tip to the sample by magnetic force.

[0035] The sample destruction unit according to this embodiment is positioned in the destruction chamber of a sample destruction device that extracts gas from inside the sample. The sample destruction unit has a tip and a holder. The tip is a separate component from the shaft provided in the sample destruction device, and destroys the sample by the kinetic force transmitted from the shaft. The holder has a sample stage on which the sample is placed, holds the tip, and guides the movement of the tip. Before sample destruction, the sample is placed between the sample stage and the tip.

[0036] The above configuration makes it easy to accurately position the tip relative to the sample. Furthermore, it eliminates problems such as sample loss during the sample transport process. Additionally, the tip and multiple fragments can be easily recovered after sample destruction. Since the tip is separated from the shaft, used tips can be replaced with other tips.

[0037] The analytical method according to this embodiment comprises steps 1 to 6. In step 1, a sample is placed on a sample stage in a holder. In step 2, a chip for destroying the sample is placed on the holder, thereby creating a state in which the sample is sandwiched between the sample stage and the chip. In step 3, a sample destruction unit having the holder and the chip is placed in the destruction chamber of the sample destruction device. In step 4, kinetic force is transmitted from a shaft provided in the sample destruction device to the chip, and the sample is destroyed by the chip. As a result, gas is extracted from the sample. In step 5, the gas extracted from the sample is analyzed. In step 6, after the gas has been extracted from the sample, the sample destruction unit is removed from the destruction chamber.

[0038] (1-2) The sample destruction apparatus according to the embodiment comprises a housing, a destruction tool, and a holder. The housing has a destruction chamber. The destruction tool destroys the sample in the destruction chamber in order to extract gas from inside the sample. The holder holds the sample. The destruction tool has a tip for destroying the sample. The holder has a guide for guiding the tip toward the sample.

[0039] According to the above configuration, the sample is held by the holder, and the movement of the tip is guided by the guides of the holder. Therefore, it becomes easy to accurately position the tip relative to the sample. If the holder or the unit containing it constitutes a portable body, the tip can be transported by transporting the portable body. Therefore, it becomes easy to set up the sample in the destruction chamber and to remove the sample from the destruction chamber.

[0040] A destructive tool generally consists of a shaft and a tip. The shaft and tip may be made of separate components, or they may be integrated. The holder and guide may be made of separate components, or they may be integrated. The guide has a channel through which gas released from the sample upon destructive destruction flows.

[0041] In the embodiment, the holder has a sample stage on which a sample is placed. The sample stage is a recess having a bottom surface on which the sample is placed. The guide has an annular lower end that is inserted into the recess. A mesh sheet is provided to cover the sample on the bottom surface. The annular lower end presses against the mesh sheet around the sample.

[0042] The sample breaking device according to this embodiment includes a magnet that generates a magnetic field that exerts a magnetic force on at least one of the sample and the chip. If the sample is magnetic, the magnetic force restricts the movement of the sample on the sample stage in the holder. If the sample has magnetic anisotropy, the magnetic force determines the position and orientation of the sample on the sample stage in the holder. If the chip is magnetic, the magnetic force applies a pressing force from the chip to the sample.

[0043] (2) Details of the embodiment Figure 1 shows an example configuration of a gas analysis system according to an embodiment. The gas analysis system extracts gas from inside a sample and analyzes the extracted gas. The gases to be analyzed include, for example, gases sealed in during the sample manufacturing process, gases that entered during the sample manufacturing process, and gases generated within the sample after the sample manufacturing process.

[0044] The sample is, for example, a small electronic device, a specific example of which is a crystal oscillator. The crystal oscillator is an ultra-small hollow package product, and its internal space is sealed. The width of the crystal oscillator is, for example, 1.0 mm, its height is, for example, 0.8 mm, and its thickness is, for example, 0.3 mm or less. The amount of gas sealed inside is extremely small. In the embodiment, the sample destruction device 10 is configured so that, after the sample is destroyed, the small amount of gas released from inside the sample is sent to the mass spectrometer without diffusing as much as possible. Note that other electronic devices or non-electronic devices may also be used as samples.

[0045] In Figure 1, the gas analysis system includes a sample breaking device 10 and a mass spectrometer 12. The sample breaking device 10 is a device that breaks a sample and extracts the gas from within. The mass spectrometer 12 is a device that performs mass analysis on the gas produced by the breakdown of the sample. Other analytical devices may be provided in place of or in addition to the mass spectrometer 12. The sample breaking device 10 and the mass spectrometer 12 are connected.

[0046] In the sample destruction device 10, the first heating block 14 is fitted with a housing 16, isolation valve 26, filter 32, isolation valve 34, etc. The housing 16 is a container surrounding the destruction chamber 18. The destruction chamber 18 is a vacuum chamber. The destruction mechanism 22 is fitted to the housing 16. The destruction mechanism 22 has a shaft 24 that moves back and forth (up and down in Figure 1). The shaft 24 is held movably by a holding member provided on the housing 16. The destruction mechanism 22 has a mechanism that converts rotational motion into linear motion. When the user rotates the knob in one direction, the shaft moves forward. When the user rotates the knob in the other direction, the shaft moves backward. An actuator to drive the shaft may be provided.

[0047] The user places the sample destruction unit 20 inside the destruction chamber 18. Specifically, a unit stage, which functions as a base, is provided inside the destruction chamber 18. The sample destruction unit 20 is placed on the unit stage. The sample destruction unit 20 holds the sample and the tip. Specifically, a sample stage is provided inside the sample destruction unit 20, and the sample is placed on the sample stage. The tip is placed on top of the sample. In other words, the sample is sandwiched between the sample stage and the tip. The tip corresponds to the tip of the destruction tool.

[0048] As the shaft 24 moves forward and collides with the tip, a kinetic force is transmitted from the shaft 24 to the tip. The forward movement of the tip causes the sample to break. For example, the sample may be crushed or cut, or a hole may be formed in the sample. The breakdown of the sample causes gas to be released from inside the sample.

[0049] An interface 36 is provided spanning the sample destruction device 10 and the mass spectrometer 12. A second heating block 15 is attached to the interface 36.

[0050] A vacuum gauge 30 is connected to the piping between the isolation valve 26 and the three-way valve 28. Port A of the three-way valve 28 is connected to the isolation valve 26 via piping, and port B of the three-way valve 28 is connected to the dry pump 50, which will be described later, via piping. Port C of the three-way valve 28 is connected to the outside. The temperature control unit 38 controls the temperatures of the first heating block 14 and the second heating block 15.

[0051] The mass spectrometer 12 has a vacuum chamber 40. Inside the vacuum chamber 40 are an ion source 42, an ion focus lens 44, a quadrupole mass spectrometer, and a detector 48. The ion source 42 is a closed ion source. In the illustrated example, a filament 43 is provided inside the ion source 42 (inside the ionization chamber).

[0052] The dry pump 50 and turbomolecular pump 52 are used to create a vacuum inside the vacuum vessel 40. In some embodiments, they are also used to create a vacuum inside the destruction chamber 18. During gas analysis, the vacuum inside the vacuum vessel 40 (especially inside the ion source 42) is higher than the vacuum inside the destruction chamber 18, resulting in a pressure difference between the two. The tip of the interface 36 is inserted into the inside of the ion source 42. A vacuum gauge 53 is connected to the vacuum vessel 40.

[0053] Note that the configuration shown in Figure 1 is merely illustrative. For example, in Figure 1, the sample may be destroyed by moving the shaft 24 in a direction other than downward (for example, upward or horizontally).

[0054] The preparation process and gas analysis process in the gas analysis system shown in Figure 1 will be described below.

[0055] First, the isolation valve 34 is closed, separating the internal space of the sample destruction device 10 from the internal space of the mass spectrometer 12. In this state, the dry pump 50 and the turbomolecular pump 52 are activated, and the inside of the vacuum chamber 40 is evacuated. Subsequently, each element of the mass spectrometer 12 is activated.

[0056] After the temperature of the second heating block 15 reaches the specified temperature due to the supply of current to the second heating block 15 and after the adjustment of the mass spectrometer 12 is completed, the sample destruction unit 20 is placed in the destruction chamber 18. Then, the front door provided on the housing 16 is closed. Subsequently, port A and port B are connected in the three-way valve 28, and the isolation valve 26 is opened. In this state, the air in the destruction chamber 18 is discharged by starting the dry pump 50. It is confirmed by the vacuum gauge 30 that the pressure in the destruction chamber 18 has reached the specified value.

[0057] Next, isolation valve 26 is closed, and isolation valve 34 is opened. In this state, the vacuum level of the destruction chamber 18 is further increased by the action of the turbomolecular pump 52. The pressure indicated by the vacuum gauge 53 is checked to confirm that it has reached the specified value.

[0058] The temperature of the first heating block 14 is controlled to heat the sample destruction unit 20 and any moisture or organic matter adhering to the sample. This causes them to volatilize and be removed. Subsequently, the mass spectrometer 12 is operated to confirm that the background ions have reached a specified state. After that, gas analysis is performed as follows.

[0059] With isolation valve 26 closed and isolation valve 34 open, the shaft is driven, and kinetic force is transmitted from the shaft to the tip. This causes the tip to collide with the sample, destroying it. This destruction releases gas from inside the sample. This gas is then drawn towards the mass spectrometer 12 due to the differential pressure.

[0060] Specifically, the gas emitted from the sample destruction unit 20 moves into the ion source 42 through the destruction chamber 18, filter 32, isolation valve 34, and interface 36. The filter 32 removes minute fragments generated from the sample. Minute fragments may also be removed by a filter equipped with an orifice.

[0061] In the ion source 42, the gas that enters it is ionized. The resulting ions enter the quadrupole mass spectrometer 46 via the ion focus lens 44. Ions with a selected mass-to-charge ratio pass through the quadrupole mass spectrometer 46 and are detected by the detector 48. A mass spectrum is generated based on the output signal of the detector 48. The components contained in the gas are analyzed by analyzing the mass spectrum.

[0062] After gas analysis, the isolation valve 34 is closed, and the temperature of the first heating block 14 is lowered. Then, the three-way valve 28 connects port A and port B, and the isolation valve 26 is opened, thereby returning the pressure in the destruction chamber 18 to atmospheric pressure. Subsequently, the front door of the destruction chamber 18 is opened, and the sample destruction unit 20 is removed from the destruction chamber 18.

[0063] The removed sample destruction unit 20 is cleaned. Specifically, multiple fragments are removed from the sample stage of the sample destruction unit 20, and the sample stage is cleaned as needed. The tip is also cleaned. If necessary, a deteriorated tip is replaced with a new one. The tip may be replaced each time the sample is destroyed.

[0064] The sample destruction device and sample destruction unit will be described in detail below.

[0065] Figure 2 shows the xz cross-section of the fracture chamber 18 in the sample fracture apparatus. Here, the x-direction is the first horizontal direction, and the z-direction is the vertical direction. The direction perpendicular to the plane of paper in Figure 2 is the y-direction, which is the second horizontal direction. The x, y, and z directions are orthogonal to each other.

[0066] The inside of the housing 16 is the destruction chamber 18. A portable sample destruction unit 20 is placed inside the destruction chamber 18. The sample destruction unit 20 holds the sample 54. More specifically, the sample destruction unit 20 consists of a main body 64, a guide 60, and a tip 56. The main body 64 and the guide 60 constitute a holder 200. The holder 200 functions as both a sample holder and a tip holder. The tip 56 is held by the guide 60, and the movement of the tip 56 is guided by the guide 60. The direction of this movement is toward the sample 54.

[0067] The shaft 24 and the tip 56 constitute the destructive tool 58. Conversely, in this embodiment, the tip 56 and the rest of the destructive tool 58 (i.e., the shaft 24) are separated. By configuring the tip 56 as an independent component, the tip 56 can be removed from the destructive chamber 18 while the shaft 24 remains attached to the housing 16. This makes cleaning the tip 56 easier. It also makes replacing the tip 56 easier.

[0068] In this embodiment, the chip 56 is placed on the sample 54 before the sample is destroyed, and the load of the chip 56 is applied to the sample 54. By restricting the movement of the sample 54, problems such as the sample 54 falling off or getting lost are less likely to occur.

[0069] The housing 16 is made of, for example, stainless steel, and the tip 56 is made of, for example, tungsten. Tungsten is a non-magnetic material. The tip 56 may also be made of, for example, stainless steel. Stainless steel is a magnetic material.

[0070] Figure 3 shows a yz cross-section of the fracture chamber in the sample fracture apparatus. The housing 16 is fixed to the first heating block 14. The first heating block 14 has a heater 78 and a temperature sensor 80 embedded in it. A unit stage 62, which functions as a base, is provided inside the housing 16. The sample fracture unit 20 is placed on the unit stage 62. The opening of the housing 16 is covered by a front door 72. The front door 72 is fixed to the housing 16 by a number of bolts 74.

[0071] In the sample breaking unit 20, a sloped surface 68 is formed on the rear of the main body 64. A leaf spring 70 is attached to the front door 72, and the tip of the leaf spring 70 contacts the sloped surface 68. Specifically, a pressing force is applied from the leaf spring 70 to the sloped surface 68 in a diagonally downward direction. This pressing force presses the sample breaking unit 20 against the rear wall surface 16A and the unit stage 62. In other words, the sample breaking unit 20 is set in the specified position.

[0072] In the sample destruction unit 20, the main body 64 has a cavity 102 into which a guide 60 is inserted. A tip 56 is inserted into the tip movement space within the guide 60.

[0073] Figure 4 shows an example of the transport device 82. The transport device 82 is used when transporting the sample destruction unit 20. Of course, the sample destruction unit may also be transported by the user.

[0074] Figure 5 shows an xz cross-section of the sample breaking unit 20. As already described, the sample breaking unit 20 has a body 64, a guide 60, and a tip 56. A sample stage 88 is formed inside the body 64. In the illustrated example, the sample stage 88 is a dish-shaped recess. The bottom surface 90 of the recess is the surface on which the sample 54 is placed. When viewed from above, the recess is, for example, circular. The depth of the recess is, for example, 0.5 to 2 mm, and its diameter is, for example, 3 to 4 mm. The body 64 and the guide 60 may be made of metal, ceramic, resin, etc.

[0075] The main body 64 has a well-shaped cavity 102 into which a guide 60 is placed. The guide 60 has an internal space for chip movement, into which a chip 56 is placed. In the guide 60, the inner surface 92 surrounds the chip movement space.

[0076] The destructive tool 58 is composed of a tip 56 and a shaft 24. The tip 56 is composed of a large-diameter portion 84 and a small-diameter portion 86 that are interconnected. The horizontal cross-sectional size of the large-diameter portion 84 is larger than that of the small-diameter portion 86. The large-diameter portion 84 is an enlarged portion, and the small-diameter portion 86 is the working portion as a convex portion. The diameter of the large-diameter portion 84 is, for example, 5 to 8 mm, and the diameter of the small-diameter portion 86 is, for example, 2 to 4 mm.

[0077] The inner surface 92 of the guide 60 has a guide surface 92A as the upper and middle portion, and an enclosing surface 92B as the lower portion. The guide surface 92A is generally cylindrical. However, the lower end of the guide surface 92A is curved inward (towards the central axis of the chip housing space). The enclosing surface 92B is cylindrical.

[0078] The large-diameter portion 84 is held and guided by the guide surface 92A. The diameter of the large-diameter portion 84 and the diameter of the guide surface 92A are approximately equal, and the side surface of the large-diameter portion 84 is in contact with the guide surface 92A. In other words, there is almost no gap between the side surface of the large-diameter portion 84 and the guide surface 92A. The small-diameter portion 86 enters the surrounding surface 92B. The diameter of the surrounding surface 92B is smaller than the diameter of the small-diameter portion 86. That is, there is a small gap between the small-diameter portion 86 and the surrounding surface 92B. The gas released from the sample 54 passes through this gap.

[0079] The guide 60 has an annular (cylindrical) projection 60A that protrudes downward and enters the sample stage 88. The projection 60A is the lower end of the annular projection. The outer diameter of the projection 60A is approximately equal to the outer diameter of the sample stage 88. The inner surface of the projection 60A is part of the surrounding surface 92B. The inner diameter of the projection 60A is larger than the diameter of the small diameter section 86. The amount of projection of the projection 60A is smaller than the depth of the sample stage 88. The amount of projection is determined so that the sample 54 can be held in place by the mesh sheet 94, which will be described below.

[0080] The upper part of the chip housing space in the guide 60 widens horizontally outward. That is, a tapered surface 93 is formed in the upper opening of the guide 60. The guide 60 has a flow channel 96 as a transverse hole and a through hole. One end of the flow channel 96 is connected to the chip housing space. When the sample destruction unit 20 is placed in the destruction chamber, the other end of the flow channel 96 is connected to the destruction chamber. The gas released from the sample 54 passes through the gaps present around the small diameter section 86 and flows into the flow channel 96.

[0081] A mesh sheet 94 is placed inside the sample stage 88. Specifically, a circular mesh sheet 94 is positioned inside the sample stage 88 so as to cover the entire sample 54 on the bottom surface 90. The mesh sheet 94 is made of a relatively soft metal, such as copper or aluminum. The annular end of the mesh sheet 94, that is, the part corresponding to the perimeter of the sample 54, is pushed downward by the lower end surface of the protrusion 60A. This causes the mesh sheet 94 to bend. However, in Figure 5, the mesh sheet is represented by a horizontal straight line. When the sample is destroyed, the chip 56 crushes the sample 54 through the mesh sheet 94 while the mesh sheet 94 is in a bent state.

[0082] The mesh sheet 94 restrains the sample 54 before sample fracture and prevents the scattering of multiple fragments generated from the sample 54 after sample fracture. The material and thickness of the mesh sheet 94 are selected so that the mesh sheet 94 does not interfere with sample fracture by the chip 56. The thickness of the mesh sheet 94 is generally less than 200 μm, preferably less than 100 or 50 μm. Multiple stacked mesh sheets 94 may be used. For example, the size and shape of each opening in the mesh sheet 94 are determined so that fragments with a size of 100 μm do not pass through the mesh sheet 94. However, the mesh sheet 94 is provided only as needed.

[0083] The sample stage 88 may have a shape other than circular, such as a square or polygon. The outer shape of the protrusion 60A is determined according to the shape of the sample stage 88. The inner shape of the protrusion 60A may also have a shape other than circular. For example, if the working end of the tip has a pointed shape, a recess or step for capturing the sample 54 may be provided on the bottom surface of the sample stage 88.

[0084] The shaft 24 has a drive end (pushing end) 24A as its lower end. The drive end 24A has a flat horizontal surface. The tip 56 has a receiving end 56A. The receiving end 56A has a flat horizontal surface. The tip 56 also has an working end 56B. Various shapes can be used for the working end 56B. In Figure 5, the working end 56B has a flat horizontal surface. The sample 54 is crushed by such a working end 56B.

[0085] Two storage chambers 98A and 98B are formed in the lower part of the main body 64. Two magnets 100A and 100B, which serve as magnetic means, are inserted inside the two storage chambers 98A and 98B. A magnetic field is formed by the two magnets 100A and 100B. The two magnets 100A and 100B attract each other by magnetic force, and there are no members provided to fix the two magnets 100A and 100B to the main body 64. The operation of the magnetic means will be described in detail later.

[0086] A single magnet may be placed, or three or more magnets may be placed. Generally, permanent magnets are used as magnets, but electromagnets may also be used.

[0087] Figure 6 shows the yz cross-section of the sample breaking unit 20. The main body 64 has a cavity 102 into which the guide 60 is fitted. The main body 64 has a sample stage 88 connected to the cavity 102. The internal space of the sample stage 88 may be understood as constituting part of the cavity 102. The sample 54 is placed inside the sample stage 88.

[0088] The guide 60 holds and guides the tip 56. The guide 60 is fixed to the main body 64 by a bracket 104. The bracket 104 is fixed to the main body 64 by a screw 106.

[0089] In this embodiment, the guide 60 has three functions. The first function is to hold and guide the tip 56. The second function is to restrain the sample through the mesh sheet 94, assuming the use of the mesh sheet 94. The third function is to guide the gas released from the sample toward the mass spectrometer.

[0090] Figure 7 is an exploded perspective view of the sample destruction unit 20. The main body 64 has two slits 102A and 102B connected to the cavity 102. For example, a tool such as tweezers can be inserted through the two slits 102A and 102B. Two magnets 100A and 100B are embedded in the lower part of the main body 64. The bracket 104 is fixed to the main body 64 by a screw 106. At the same time, the guide 60 is fixed to the main body 64. The chip 56 is dropped into the chip housing space of the guide 60. Figure 8 shows the assembled sample destruction unit 20. The receiving end 56A of the chip 56 is exposed.

[0091] Figure 9 schematically shows the magnetic field formed by two magnets 100A and 100B used as magnetic means.

[0092] If the sample 54 is magnetic, a magnetic force acts on the sample 54 when it is placed in a magnetic field, causing the sample 54 to stick to the bottom surface 90 of the sample stage. This restricts the movement of the sample 54. In this case, from the viewpoint of restraining the sample 54, it is not necessary to provide a mesh sheet.

[0093] If the tip 56 is magnetic, a magnetic force acts on the tip 56 when it is placed in a magnetic field, and the tip 56 is pulled towards the sample 54. The pressing force exerted by the tip 56 on the sample 54 is increased by the magnetic force. This allows the sample 54 to be restrained more securely.

[0094] A miniature hollow package containing electronic elements typically consists of a package body and a lid (LID). The package body is usually made of ceramic. While lids made of ceramic are sometimes used, recently, lids made of Kovar material have become commonly used. According to the inventors' experiments, a lid made of Kovar material exhibits magnetic polarization in its longitudinal or rolling direction in a magnetic field. In other words, a lid made of Kovar material has magnetic anisotropy.

[0095] When a miniature package product containing Kovar material is placed on the bottom surface 90 as sample 54, the package product is localized to a specific position (center) while maintaining a specific orientation due to magnetic force (see F1, F2, F3). Conversely, if the sample has magnetic anisotropy, the position and orientation of one or more magnets are adjusted so that the sample is localized to the desired position and orientation.

[0096] Figure 10 shows a chipset consisting of multiple types of chips (A) to (I). Each chip (A) to (I) is composed of a large diameter portion 108 and a small diameter portion 110. In the multiple types of chips (A) to (I), the shape of the large diameter portion 108 is the same, while the shape of the small diameter portion 110 differs. In particular, the shapes of the working ends 110A to 110I are different.

[0097] The working end 110A has a flat shape. The working end 110B has a hemispherical shape. The working end 110C has a frustoconical shape. The working end 110D has a conical shape. The working end 110E has multiple columnar projections. The working end 110F has multiple sharp projections. The working end 110G has a pin protruding forward. The working end 110H has a V-shaped groove. The working end 110I has a rectangular groove. Depending on the sample, and especially depending on the size and material of the sample, the tip to be used is selected from the tip set.

[0098] Figure 11 is a flowchart illustrating the analysis method according to the embodiment. In S10, a chip is selected from the chipset according to the sample. In S12, the sample destruction unit is assembled. Specifically, the sample is placed on the bottom surface of the sample stage in the main body, and then, if necessary, a mesh sheet is placed inside the sample stage. After that, a guide is placed on the main body and fixed to the main body with a bracket. Then, a chip is placed inside the guide. The chip may be placed inside the guide before the guide is fixed.

[0099] In S14, the sample destruction unit is placed inside the destruction chamber. Note that Figure 11 omits the illustration of the process for preparing the mass spectrometer and sample destruction device for operation.

[0100] In S16, the sample is destroyed by a destructive device. Specifically, the sample is destroyed by driving a shaft and applying kinetic force from the shaft to the tip. As the sample is destroyed, gas is released from inside the sample. This gas moves from the sample destruction device to the mass spectrometer. In S18, the gas is analyzed in the mass spectrometer.

[0101] In S20, the sample destruction unit is removed from the destruction chamber. The sample destruction unit is then disassembled, and the sample stage and tip are cleaned.

[0102] Figure 12 shows a modified sample destruction unit. The sample destruction unit 112 has a main body 114 and a guide 116. A sample stage 120 is provided at the bottom of the main body 114. A dish-shaped recess 124 is formed on the bottom surface of the sample stage 120. A sample 126 is placed in this recess 124. A mesh sheet is placed inside the sample stage 120 so as to cover the sample 126.

[0103] The guide 116 has a chip housing space. The chip housing space is surrounded by an inner surface 122. The inner surface 122 has an upper guide surface 122A and a lower guide surface 122B. A cylindrical projection 118 is formed at the lower part of the guide 116, and the projection 118 is inserted into the sample stage 120.

[0104] In Figure 12, the chip is composed of two independent components, namely ball 128 and ball 130. The diameter of ball 128 is larger than the diameter of ball 130. Ball 128 is held and guided by guide surface 122A. Ball 130 is held and guided by guide surface 122B. Ball 128 rests on ball 130, and the central axes of the two balls 128 and 130 coincide. These central axes coincide with the center of the sample. A passage such as a groove is provided to connect the space within the sample stage 120 and the chip housing space, but its illustration is omitted.

[0105] The shaft strikes ball 128, and kinetic force from the shaft is transferred to ball 128. Ball 128 strikes ball 130, and kinetic force is transferred from ball 128 to ball 130. As a result, ball 130 crushes sample 126. Sample 126 is trapped by the depression 124, and even when the lower end of ball 130 strikes sample 126, sample 126 does not escape horizontally.

[0106] Each ball 128,130 is made of ceramic, sapphire, tungsten, etc. Various forms other than balls can be used as multiple elements corresponding to the tip. According to the configuration shown in Figure 12, it is possible to replace only the part of the tip that has deteriorated and worn (i.e., ball 130).

[0107] Figure 13 shows a first example of a unit exchange mechanism provided in a sample destruction device. Reference numeral 134 indicates multiple sample units, numbered 1 to 5. The unit exchange mechanism 136 is a mechanism for sliding multiple sample units. Reference numeral 138 indicates a destruction tool consisting of a shaft and a tip. However, the tip is part of the sample unit. Each sample unit is sequentially fed into the destruction chamber 132 or sequentially positioned below the shaft. This allows multiple samples to be destroyed sequentially.

[0108] Figure 14 shows a second example of a unit exchange mechanism provided in a sample destruction device. Reference numeral 146 indicates multiple sample units, numbered 1 to 3. The unit exchange mechanism 144 is a mechanism for transporting multiple sample units. Specifically, multiple sample units are placed on a turntable 142. The unit exchange mechanism 144 is a mechanism for rotating the turntable 142. Reference numeral 148 indicates a destruction tool consisting of a shaft and a tip. However, the tip is part of the sample unit. Each sample unit is positioned sequentially below the shaft. This allows multiple samples to be destroyed in sequence.

[0109] Figure 15 shows a modified gas analysis system. The gas analysis system consists of three sample breaking devices 154, 156, and 158 and one mass spectrometer 150. Each sample breaking device has the same configuration as the sample breaking device shown in Figure 1. The three sample breaking devices 154, 156, and 158 are connected to the ion source 152 in the mass spectrometer 150 via three interfaces 160, 162, and 164. The three sample breaking devices 154, 156, and 158 operate in sequence, and the three gases they generate are sequentially introduced into the ion source 152. These gases are then analyzed in sequence.

[0110] According to the above embodiment, the sample can be reliably destroyed and the gas inside it can be extracted. Furthermore, since the space in which the gas diffuses or flows is restricted, the gas can be analyzed with high sensitivity.

[0111] In the above embodiment, the shaft is a member that imparts kinetic force to the tip. Various types of shafts can be used. For example, a shaft that transmits rotational kinetic force instead of linear kinetic force, or a shaft that transmits both linear and rotational kinetic force may be provided. A shaft that functions like a lever may be provided. A shaft equipped with a first engagement structure may be used. The first engagement structure engages with a second engagement structure provided on the tip. The above holder or sample breaking unit enables the tip to be accurately positioned relative to the sample and facilitates the handling of the sample. From this viewpoint, the shaft and tip constituting the breaking tool may be integrated. [Explanation of Symbols]

[0112] 10 Destruction device, 12 Mass spectrometer, 18 Destruction chamber, 20 Sample destruction unit, 24 Shaft, 54 Sample, 56 Tip, 58 Destruction tool, 60 Guide, 64 Main unit, 88 Sample stage, 94 Mesh sheet, 100A, 100B Magnet.

Claims

1. A housing with a destruction chamber, Within the aforementioned destruction chamber, a destruction tool is used to destroy the sample in order to extract gas from inside the sample, Includes, The aforementioned destructive device is A shaft held movably by the housing, A component separate from the shaft, comprising a chip that destroys the sample by the kinetic force transmitted from the shaft, including, A sample destruction device characterized by the following features.

2. In the sample destruction apparatus according to claim 1, The aforementioned shaft has a drive end, The aforementioned chip is A receiving end that receives the kinetic force from the driving end, An operating end that applies the aforementioned kinetic force to the sample to destroy the sample, Having A sample destruction device characterized by the following features.

3. In the sample destruction apparatus according to claim 2, It includes multiple chips, each having multiple different operating ends. The chip used to destroy the sample is a chip selected from the plurality of chips. A sample destruction device characterized by the following features.

4. In the sample destruction apparatus according to claim 1, Includes a holder that holds the sample and the chip, The holder and the tip constitute a sample destruction unit. The sample destruction unit is installed in the destruction chamber before sample destruction and removed from the destruction chamber after sample destruction. A sample destruction device characterized by the following features.

5. In the sample destruction apparatus according to claim 4, The aforementioned holder is, A body having a cavity, A guide is placed within the cavity and guides the movement of the tip, Includes, The main body includes a sample stage facing the cavity, Before the sample is destroyed, the sample is sandwiched between the sample stage and the tip. A sample destruction device characterized by the following features.

6. In the sample destruction apparatus according to claim 5, The guide has a channel through which gas released from the sample upon destruction of the sample flows. A sample destruction device characterized by the following features.

7. In the sample destruction apparatus according to claim 5, The sample stage is a recess having a bottom surface on which the sample is placed. The guide has an annular lower end that is inserted into the recess, A mesh sheet is provided to cover the sample on the bottom surface. The annular lower end presses against the mesh sheet around the sample. A sample destruction device characterized by the following features.

8. In the sample destruction apparatus according to claim 4, Includes a magnet that generates a magnetic field that exerts a magnetic force on at least one of the sample and the chip, A sample destruction device characterized by the following features.

9. In the sample destruction apparatus according to claim 8, The aforementioned sample has magnetism, The magnetic force restricts the movement of the sample on the sample stage in the holder. A sample destruction device characterized by the following features.

10. In the sample destruction apparatus according to claim 9, The aforementioned sample has magnetic anisotropy, The position and orientation of the sample on the sample stage are determined by the magnetic force. A sample destruction device characterized by the following features.

11. In the sample destruction apparatus according to claim 8, The aforementioned chip has magnetism, The magnetic force applies a pressing force from the tip to the sample. A sample destruction device characterized by the following features.

12. A sample destruction unit, which is placed inside the destruction chamber of a sample destruction device that extracts gas from the inside of a sample, A component separate from the shaft provided in the aforementioned sample destruction device, comprising a tip that destroys the sample by the kinetic force transmitted from the shaft, A sample stage on which the aforementioned sample is placed, a holder that holds the chip and guides the movement of the chip, Includes, Before the sample is destroyed, the sample is placed between the sample stage and the chip. A sample destruction unit characterized by the following features.

13. The process of placing the sample on the sample stage in the holder, A step of placing a chip for destroying the sample on the holder, thereby creating a state in which the sample is sandwiched between the sample stage and the chip, A step of placing the sample destruction unit having the holder and the tip into the destruction chamber of the sample destruction device, The process involves transmitting kinetic force from a shaft provided in the sample destruction device to the tip, thereby destroying the sample with the tip, and thereby extracting gas from within the sample. A step of analyzing the gas extracted from the sample, After the gas is removed from the sample, the sample destruction unit is removed from the destruction chamber. An analytical method characterized by including [a certain component].

14. A housing with a destruction chamber, Within the aforementioned destruction chamber, a destruction tool is used to destroy the sample in order to extract gas from inside the sample, A holder for holding the sample, Includes, The destructive tool has a chip for destroying the sample, The holder has a guide that guides the tip toward the sample. A sample destruction device characterized by the following features.

15. In the sample destruction apparatus according to claim 14, The guide has a channel through which gas released from the sample upon destruction of the sample flows. A sample destruction device characterized by the following features.

16. In the sample destruction apparatus according to claim 14, The holder has a sample stage on which the sample is placed, The sample stage is a recess having a bottom surface on which the sample is placed. The guide has an annular lower end that is inserted into the recess, A mesh sheet is provided to cover the sample on the bottom surface. The annular lower end presses against the mesh sheet around the sample. A sample destruction device characterized by the following features.

17. In the sample destruction apparatus according to claim 14, Includes a magnet that generates a magnetic field that exerts a magnetic force on at least one of the sample and the chip, A sample destruction device characterized by the following features.

18. In the sample destruction apparatus according to claim 17, The aforementioned sample has magnetism, The magnetic force restricts the movement of the sample on the sample stage in the holder. A sample destruction device characterized by the following features.

19. In the sample destruction apparatus according to claim 18, The aforementioned sample has magnetic anisotropy, The magnetic force determines the position and orientation of the sample on the sample stage in the holder. A sample destruction device characterized by the following features.

20. In the sample destruction apparatus according to claim 17, The aforementioned chip has magnetism, The magnetic force applies a pressing force from the tip to the sample. A sample destruction device characterized by the following features.

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