Sample container and elemental analyzer

By designing a sample container with cylindrical sidewalls, a surface for sample pressing, a gas channel during heating, and a hook feature that can automatically remove hook features, the problem of poor stability of irregularly shaped solid samples in elemental analysis is solved, and the stable storage and automated operation of samples are achieved, which improves the reliability and accuracy of the analysis results.

JP7673066B2Active Publication Date: 2025-05-08HORIBA LTD
View PDF 3 Cites 0 Cited by

Patent Information

Application Number
JP2022532496
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-06-26
Filing Date
2021-06-22
Publication Date
2025-05-08
Estimated Expiration
2041-06-22

AI Technical Summary

Technical Problem

In the prior art, it is difficult to stabilize the processing of irregularly shaped solid samples when performing elemental analysis, resulting in poor stability of the samples in the heating furnace, difficult to achieve automated operations, and the reliability and consistency of the analysis results are affected.

Method used

A sample container with cylindrical side walls, a surface for pressing the sample, a gas channel during heating and an automatic hook feature is designed. Through its cylindrical structure and specific channels and hook design, the container is able to stably store and process irregularly shaped solid samples and control the gas channels during heating to improve combustion efficiency.

Benefits of technology

This sample container can effectively and stably store and process irregularly shaped solid samples, improve the stability of the sample in the heating furnace, realize the reliability of automated operations and the consistency of analysis results, and at the same time, by delaying the start time of sample combustion, the generation of contaminated elements is reduced and the accuracy of analysis is improved.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure 0007673066000001
    Figure 0007673066000001
  • Figure 0007673066000002
    Figure 0007673066000002
  • Figure 0007673066000003
    Figure 0007673066000003
Patent Text Reader

Abstract

In order to provide a sample container capable of receiving even a solid sample of an irregular shape if the sample has a size insertable into a heating furnace and facilitating insertion into / pulling out from the heating furnace, this sample container 100 is used for an element analysis device 200 for heating a sample W and for extracting and analyzing a component gas, and is to be inserted into a heating furnace Z1 included in the element analysis device 200 with the sample W housed therein, the sample container 100 comprising at least: a cylindrical lateral wall 1 formed in a substantially hollow cylindrical shape; a pressed surface 3 to be pressed by a rod Y221 during insertion into heating furnace Z1; and a ventilation hole 4 through which gas passes during heating of the sample W. The sample container is provided with an end surface 2 provided to one end of the cylindrical lateral wall 1; and a hook 5 which is provided to the one end of the cylindrical lateral wall 1 and on which the rod is hooked during extraction from the heating furnace Z1.
Need to check novelty before this filing date? Find Prior Art

Description

[Technical field]

[0001] The present invention relates to a sample container used in an elemental analyzer that heats a sample to extract and analyze component gases. [Background technology]

[0002] For example, elemental analyzers are used to analyze inorganic elements such as carbon (C) and sulfur (S) contained in samples such as various metals and ceramics.

[0003] In such an elemental analysis device, for example, a powdered sample is placed in a boat-shaped ceramic sample container and inserted into a cylindrical heating furnace extending horizontally, and then the sample is heated and burned while supplying oxygen to extract the component gases (see Patent Document 1). The sample container is pushed into the heating furnace by, for example, a rod of an automatic machine, and after the analysis is completed, the rod is hooked onto a part of the sample container and pulled out of the heating furnace.

[0004] However, when an amorphous solid sample cannot be accommodated in a boat-shaped sample container, the solid sample itself is directly inserted into the heating furnace without using a sample container. Such elemental analysis without using a sample container has several problems, as follows:

[0005] 1. When the size and shape of the sample are not uniform and it is difficult to handle it with a rod or the like, it is difficult to hold the sample stably when inserting it into the heating furnace, especially when using an automated machine.

[0006] 2. It is difficult to automate the insertion and removal of samples, so it is difficult to keep the time it takes to insert the sample into the furnace or to remove the sample from the furnace constant, thereby keeping the sample combustion time constant, which causes variations in the results of elemental analysis.

[0007] 3. If the sample can be accommodated in a sample container, it can be inserted into the heating furnace with certainty. However, if the sample is to be placed directly into the heating furnace, it is necessary to select in advance whether the sample can actually be inserted into the heating furnace. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Japanese Patent Application Publication No. 6-273288 Summary of the Invention [Problem to be solved by the invention]

[0009] The present invention aims to solve all of the problems mentioned above at once, and aims to provide a sample container that can accommodate even amorphous solid samples as long as they are small enough to be inserted into a heating furnace, and can be easily inserted and removed from the heating furnace. [Means for solving the problem]

[0010] In other words, the sample container of the present invention is used in an elemental analysis apparatus which heats a sample and extracts and analyzes its component gases, and is a sample container which is inserted into a heating furnace of the elemental analysis apparatus with the sample contained therein, and which at least comprises a cylindrical side wall having a roughly hollow cylindrical shape, a pressed surface which is pressed by a rod when the sample is inserted into the heating furnace, and an air hole through which gas passes when the sample is heated, and is characterized in having an end surface portion provided at one end of the cylindrical side wall, and a hook portion provided at the one end of the cylindrical side wall on which a rod is hooked when the sample is removed from the heating furnace.

[0011] In this case, since the space for accommodating the sample can be made larger within the cylindrical side wall than in the conventional boat-shaped sample container, for example, the sample can be easily accommodated inside, even if it is a solid sample of an irregular shape. Therefore, even samples of shapes and sizes that would have been inserted directly into the heating furnace in the conventional case can be accommodated in the sample container. As a result, the stability of the holding state of the sample when the sample is inserted into or removed from the heating furnace can be improved.

[0012] In addition, since the sample is accommodated in the sample container regardless of its shape, it can be easily handled by an automated machine. This makes it possible to keep the time it takes to move the sample container in and out of the heating furnace constant, thereby making it possible to keep the sample heating time constant and suppressing variation between analyses.

[0013] Furthermore, since the sample is contained in a state covered by the cylindrical side wall, the sample is less likely to be directly heated compared to a boat-type sample container with a large opening on the top surface, and the time when the sample starts to burn can be delayed compared to the conventional method. Therefore, elements that cause contamination and are attached to the sample container can be sufficiently heated and desorbed before the sample burns and the component gases are generated. Therefore, it is possible to prevent almost no contamination from occurring at the stage when the sample burns and the component gases are generated, and it is possible to improve the accuracy of the analysis.

[0014] In addition, by changing the size and position of the vent hole and the shape of the cylindrical side wall itself, the direction of the combustion gas for burning the sample can be changed, and as a result, the burning speed of the sample can be improved compared to the conventional method.

[0015] In addition, if the sample can be accommodated in the sample container, there is no need to select the size or other factors required to determine whether the sample can be inserted into the heating furnace, as is the case when the sample is directly inserted into the heating furnace.

[0016] In order to make it easy for an automated machine to hook a rod to the sample container in the heating furnace and pull it out while making the volume of the sample storage space in the cylindrical side wall as large as possible, the vent hole should be large enough to allow a part of the rod to pass through, and the hooked part should be the inner surface of the sample container at the end face. In this case, the hooked part is located at a predetermined position regardless of the circumferential orientation of the sample container in the heating furnace, making it easy for an automated machine to hook a rod to the sample container.

[0017] In order to form the largest possible storage space for the sample, the heating furnace should have a furnace body that is approximately hollow cylindrical in shape and has a predetermined inner diameter, and the cylindrical side wall should be approximately hollow cylindrical in shape and have outer dimensions that are approximately the same as the inner diameter of the furnace body.

[0018] To make it easier to insert the sample into the cylindrical side wall, a sample insertion port for inserting the sample into the sample container opens at the other end of the cylindrical side wall, and the inner diameter dimension of the sample insertion port is formed to be larger than the inner diameter dimension of the air hole.

[0019] In order to prevent the rod from coming into contact with the sample when the sample container is inserted into the heating furnace, which may result in contamination, etc., it is sufficient to further include an intrusion prevention member provided on the one end side within the cylindrical side wall to prevent the rod inserted through the air hole from intruding beyond a specified position toward the other end side.

[0020] In order to prevent the same elements as the component gas to be analyzed from adhering to the sample container and to reduce the effect of contamination on the analysis results, it is sufficient that at least the outer or inner peripheral surface of the cylindrical side wall is metal plated.

[0021] In order to reduce the thermal conductivity of the sample container and delay the time when the sample starts to burn compared to conventional methods, while also making it easier to visually observe the internal state of the sample, it is sufficient that at least the cylindrical side wall is made of quartz glass.

[0022] An elemental analysis apparatus equipped with a sample container according to the present invention and a heating furnace having a cylindrical furnace body having at least a portion of an inner diameter dimension that is approximately the same as the radial outer diameter dimension of at least a portion of the cylindrical side wall of the sample container makes it possible to perform more accurate elemental analysis even with, for example, an amorphous solid sample that would previously have been directly inserted into the heating furnace. Effect of the Invention

[0023] In this way, the sample container according to the present invention can stably hold an amorphous solid sample in the storage space in the cylindrical side wall. This makes it easy to handle using an automated machine, and the time required to insert the sample into the heating furnace can be made constant, thereby reducing the variation in analysis. In addition, since the sample can be heated while almost entirely covered by the sample container, the start time of the combustion of the sample can be delayed compared to the conventional method. As a result, elements attached to the sample container that cause contamination can be desorbed and removed before the generation of component gases, thereby improving the accuracy of analysis. [Brief description of the drawings]

[0024] [Figure 1] FIG. 1 is a schematic diagram showing a configuration of an elemental analyzer according to an embodiment of the present invention. [Diagram 2] FIG. 2 is a perspective view of a sample container used in the elemental analyzer of the embodiment. [Diagram 3] 3A to 3C are six-sided views of a sample container used in the elemental analyzer of the embodiment. [Figure 4] FIG. 4 is a schematic perspective view showing a hand for transporting a sample container in the embodiment; [Diagram 5] 5A and 5B are schematic diagrams showing insertion and removal of a sample container into and from a heating furnace in the embodiment; [Figure 6] FIG. 13 is a perspective view of a sample container used in the elemental analyzer of another embodiment. [Figure 7] 6A and 6B are six-sided views of a sample container used in an elemental analyzer according to another embodiment. [Figure 8] FIG. 13 is a schematic diagram showing a furnace body and a sample container according to still another embodiment. [Figure 9] FIG. 13 is a schematic diagram showing a modified example of a metal-plated sample container. [Figure 10] FIG. 2 is a schematic diagram illustrating a method for elemental analysis using multiple heating stages. [Figure 11] Graph showing the relationship between the material of the sample container and the amount of CO2 generated in a blank measurement. [Explanation of symbols]

[0025] 200...Elemental analyzer 200X Stocker unit X1 Storage shelf X2 Handling mechanism 200Y Supply unit Y1...1st supply mechanism Y2...Second supply mechanism 200Z...Analysis unit Z1...Heating furnace W: Sample 100...container 1. Cylindrical side wall 2...End face part 3. Pressed surface 4. Ventilation holes 5 Hooked part 6 Sample insertion port 7. Intrusion prevention member DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0026] Hereinafter, a sample container 100 used in an elemental analyzer 200 according to an embodiment of the present invention will be described with reference to the accompanying drawings.

[0027] <Device configuration>

[0028] The elemental analysis apparatus 200 of this embodiment heats and combusts a sample W such as a metal, and analyzes elements contained in the sample W, such as carbon (C) and sulfur (S), from the component gases produced by the combustion.

[0029] This elemental analysis apparatus 200 includes a storage unit 200X in which a plurality of sample containers 100 containing samples W are stocked, an analysis unit 200Z which heats the sample containers 100 inserted into a heating furnace Z1 and performs elemental analysis of the component gases extracted from the sample W, and a container supply unit 200Y which automatically supplies one of the sample containers 100 from the storage unit 200X to the analysis unit 200Z and also loads and unloads the sample container into the heating furnace Z1.

[0030] The analytical unit 200Z includes a heating furnace Z1 in which a sample container 100 is placed, and a gas analyzer Z4 that analyzes component gases generated from a sample W heated and combusted in the heating furnace Z1, as shown in FIG.

[0031] The sample container 100 accommodates, for example, an amorphous solid sample W therein, and the sample container 100 of this embodiment has a generally hollow cylindrical shape as shown in Figures 2 and 3. The details of the sample container 100 will be described later.

[0032] As shown in FIG. 1, the heating furnace Z1 is used to heat a sample container 100 that does not contain a sample W therein, or to heat a sample container 100 that contains a sample W therein.

[0033] Specifically, the heating furnace Z1 has a space Z3S extending horizontally from an opening Z3H formed in a side wall, and the sample container 100 is placed in the space Z3S, and includes a furnace body Z31 into which the sample container 100 is inserted and removed, an electric resistor Z12 provided around the furnace body Z31 to heat the furnace body Z31, and a power supply circuit Z13 that supplies power to the electric resistor Z12 to generate heat. In this embodiment, the opening Z3H is formed in the front wall of the heating furnace Z1, and a roughly cylindrical space Z3S is formed in the depth direction from the opening Z3H.

[0034] The furnace body Z31 is, for example, a cylindrical ceramic molded body, and has a space Z3S inside which the sample container 100 can be accommodated. One end of the furnace body Z31 communicates with the opening Z3H. The other end of the furnace body Z31 is provided with a gas outlet for guiding the gas generated from the sample W to the gas analyzer Z4. The furnace body Z31 may be heated by passing an electric current through an electric resistance furnace to perform resistance heating (Joule heating), in which case the furnace body Z31 is made of a metal having electrical conductivity. Alternatively, the sample container 100 or the sample W accommodated in the furnace body Z31 may be induction heated.

[0035] The gas analyzer Z4 analyzes the component gases generated in the heating furnace Z1 to determine the content of each component contained in the sample W. In this embodiment, the analysis is performed using, for example, a non-dispersive infrared absorption method (NDIR method). Specifically, the gas analyzer Z4 has a non-dispersive infrared detector (not shown) and detects CO 2 , CO, SO 2 By detecting these, the amount of carbon (C), sulfur (S), etc. contained in the sample W can be determined.

[0036] In this embodiment, the heating furnace Z1 and the gas analyzer Z4 are unitized to form one analysis unit 200Z. This analysis unit 200Z may be configured to be movable by casters or the like.

[0037] The stocker unit 200X includes, for example, a storage shelf X1 having multiple shelves on which multiple sample containers 100 are placed, and a handling mechanism X2 that picks up one of the sample containers 100 from the storage shelf X1 and moves it to a receiving position P in the container supply unit 200Y. This stocker unit 200X may also be configured to be movable by casters or the like.

[0038] The handling mechanism X2 includes a hand X21 that lifts a generally cylindrical sample container 100 from below as shown in FIG. 4. The hand X21 includes two support members X211 that support the outer side of the sample container 100 from below, and a plate-shaped cover X213 that is disposed at a predetermined distance from both ends of the sample container 100 and prevents the sample W in the sample container 100 from leaking out from both ends. A V-shaped groove X212 on which the cylindrical sample container 100 is placed is formed in the center of each support member X211. In this manner, when the sample container 100 is placed on the hand X21, the sample container 100 can rotate around a horizontal axis, but the sample W can be transported in a stable state so that it does not leak out of the sample container 100.

[0039] As shown in FIG. 1(b), the container supply unit 200Y receives the sample container 100 from the stocker unit 200X and supplies the sample container 100 through an opening Z3H formed in the side wall of the heating furnace Z1. Specifically, the container supply unit 200Y is provided to relay between the stocker unit 200X and the analysis unit 200Z. The container supply unit 200Y also includes a first container supply mechanism Y1 configured to move the sample container 100 from a receiving position P of the sample container 100 adjacent to the stocker unit 200X to a waiting position Q set outside the heating furnace Z1, and a second container supply mechanism Y2 configured to move the sample container 100 from the waiting position Q to a combustion position R set inside the heating furnace Z1. In this embodiment, the moving direction of the sample container 100 from the receiving position P to the waiting position Q and the moving direction of the sample container 100 from the waiting position Q to the combustion position R are configured to be perpendicular to each other in a horizontal plane. The attitude of the sample container 100 is kept constant during the movement.

[0040] 1(a), the first container supply mechanism Y1 moves the sample container 100 horizontally from a receiving position P to a waiting position Q, and is, for example, a moving table equipped with a motor, a ball screw, a table, and a guide. Here, the waiting position Q is a position where the sample container 100 is set just before being heated, and in this embodiment, it is set in front of the entrance of the heating furnace Z1.

[0041] The second container supply mechanism Y2 includes an actuator Y22 that pushes the sample container 100 horizontally as shown in Figure 1(b), a horizontal movement unit Y1 consisting of an actuator such as a motor or an air cylinder that drives the actuator Y22, and a lifting unit Y23 that includes a linear guide mechanism extending vertically and an actuator such as a motor or an air cylinder, and raises and lowers the horizontal movement unit Y1 vertically.

[0042] In this embodiment, the actuator Y22 may linearly advance and retreat, or may linearly expand and contract. The actuator Y22 also functions as an insertion rod for inserting the sample container 100 into the heating furnace Z1, and as a pull-out rod for pulling the sample container 100 out of the heating furnace Z1. A hook Y221 is formed at the tip of the actuator Y22 to be hooked when pulling out the sample container 100.

[0043] When the sample container 100 is inserted into the furnace body Z31 of the heating furnace Z1, the vertical position of the actuator Y22 is adjusted by the lifting unit Y23 so that the actuator Y22 contacts the outer edge of the end face 2 of the sample container 100. When the sample container 100 is pulled out of the heating furnace Z1, the height of the actuator Y22 is adjusted by the lifting unit Y23 so that the hook portion Y221 hooks onto a part of the sample container 100.

[0044] The container supply unit 200Y further includes a disposal mechanism Y3 for disposing of the sample container 100 after the analysis. The disposal mechanism Y3 disposes of the container heated by the heating furnace Z1, and includes a disposal section Y31 having an opening at the top, an opening / closing lid Y32 for closing the opening of the disposal section Y31, and an actuator (not shown) for opening and closing the opening by lowering the opening / closing lid Y32. Here, the sample container 100 drawn out from the heating furnace Z1 is placed on the top surface of the opening / closing lid Y32, and is disposed of in the disposal section Y31 by lowering the opening / closing lid Y32 by the actuator. The disposal section Y31 may be a container, or may be a disposal flow path connected to an external disposal container (not shown).

[0045] In this embodiment, the first container supply mechanism Y1, the second container supply mechanism Y2, and the disposal mechanism Y3 are unitized to configure one container supply unit 200Y. The supply unit 200Y is configured to be movable by casters or the like. The supply unit 200Y is configured to be detachable from the analysis unit 200Z or the stocker unit 200X.

[0046] Next, the sample container 100 will be described in detail with reference to FIGS.

[0047] The sample container 100 has a generally hollow cylindrical shape as shown in Fig. 2 and Fig. 3, and contains a lump of sample W having a predetermined volume inside. The sample container 100 is transparent and made of, for example, quartz glass, so that the sample W contained inside can be seen from the outside. The material of the sample container 100 is not limited to quartz glass, and may be other materials such as ceramics. In Fig. 2 and Fig. 3, the outer ridges or contours of the sample container 100 are drawn with solid lines, and the inner ridges, valleys, and contours are drawn with dotted lines. In Fig. 2 and Fig. 3, the end surface portion 2 pushed and pulled by the actuator Y22 of the supply unit 200Y is drawn as the front.

[0048] The sample container 100 is generally thin-walled and hollow, and includes a cylindrical side wall 1 having a storage space for storing a sample W therein, an end surface portion 2 provided at one end of the cylindrical side wall 1, and a sample insertion port 6 opening at the other end of the cylindrical side wall 1 and through which the sample W is inserted into the storage space. The diameter of the sample insertion port 6 is set to, for example, 25 mm, and is larger than the vent hole 4 described below. As shown in Fig. 4, the outer diameter of the cylindrical side wall 1 of the sample container 100 is set to be approximately the same as the inner diameter of the heating furnace Z1.

[0049] The end surface portion 2 is open at the center, and as shown in FIG. 5(b), oxygen (O 2) is provided. Around the vent hole 4 on the outside of the end surface 2, a circular pressed surface 3 is formed which is pressed by the tip of the rod, which is the actuator Y22, when the sample container 100 is inserted into the heating furnace Z1, as shown in FIG. 5(a). Around the vent hole 4 on the inside of the end surface 2, a circular pressed surface 3 is formed which is pressed by the tip of the rod, which is the actuator Y22, when the sample container 100 is pulled out from the heating furnace Z1, as shown in FIG. 5(c). Specifically, the diameter of the vent hole 4 is set to a size that allows the hook part Y221 of the rod to pass through, and is set to a diameter of, for example, 13 mm. After the hook part Y221 is inserted into the sample container 100, the actuator Y22 moves radially outward, so that the hook part Y221 is hooked onto the hook part 5.

[0050] Furthermore, inside the sample container 100, an intrusion prevention member 7 is provided at one end side (end surface portion 2 side) to prevent the rod from intruding beyond that position toward the other end side (insertion port 6 side). This intrusion prevention member 7 is a cylindrical member extending radially inside the sample container 100, and is arranged so as to overlap with the vent hole 4 when viewed from the front side as shown in the front view of FIG. 3. That is, even if a rod which is the actuator Y22 is inserted from the vent hole, it will interfere with this intrusion prevention member 7, so that the rod will not interfere with the sample W contained inside. Also, the periphery of the intrusion prevention member 7 is left hollow so as not to block the inside of the storage space.

[0051] <Effects of this embodiment>

[0052] According to the sample container 100 of this embodiment, a large storage space for storing the sample W can be formed inside the cylindrical side wall 1, so that even if the sample W is, for example, a solid sample with an irregular shape, it is easy to store it inside. Therefore, even if the sample W has a shape and size that would have been directly inserted into the heating furnace Z1 in the past, it can be stored in the sample container 100 in a stably held state.

[0053] In addition, the outer shape of the sample container 100 is formed to be cylindrical and almost the same as the cylindrical furnace body 31 of the heating furnace Z1, so that when the sample container 100 is inserted into the heating furnace Z1, the sample container 100 is naturally guided along the axial direction. This improves the stability of the holding state of the sample W when the sample container 100 is inserted into or removed from the heating furnace Z1, and improves the stability of handling by the second container supply mechanism Y2. This makes it possible to keep the time required for the sample container 100 to be inserted and removed from the heating furnace Z1 constant, thereby making it possible to keep the heating time of the sample W constant and suppressing variation between analyses.

[0054] Furthermore, since the sample W is accommodated in the cylindrical side wall 1 with the entire circumference covered, and the sample container 100 is made of quartz glass, the sample W is less likely to be directly heated compared to a boat-shaped sample container 100 with a large opening on the top. Also, since the sample container 100 is made of quartz glass, which has a large heat capacity and is a material that does not easily conduct heat, the start time of combustion of the sample W can be delayed compared to the conventional method. That is, the sample container 100 can be heated sufficiently and the sample W can start to burn after, for example, the element to be analyzed that is attached to the cylindrical side wall 1 is sufficiently desorbed. Therefore, it becomes easier to remove contamination from the component gas extracted from the sample W, and the analysis accuracy by the analysis unit 200Z can be improved.

[0055] Furthermore, since the sample container 100 can only rotate in the circumferential direction within the furnace body Z31, the orientation and posture of the hook portion 5 formed as the inner surface of the end face portion 2 do not change, and it can be reliably maintained in a state where it can be easily hooked onto the hook portion Y221 of the rod, which is the actuator Y22.

[0056] In addition, unlike the case of direct insertion, there is no need to select the size or the like to determine whether or not the material can be inserted into the heating furnace Z1.

[0057] <Other Modified Embodiments>

[0058] The present invention is not limited to the above-described embodiment.

[0059] As shown in FIGS. 6 and 7, the sample container 100 may not be provided with an intrusion prevention member 7.

[0060] As shown in FIG. 8(a) and FIG. 8(b), the cylindrical side wall 1 of the sample container 100 does not have to be cylindrical in its entirety. For example, the outer peripheral surface of the end portion opposite to the end surface portion, which is disposed on the elemental analyzer Z4 side, may be tapered. That is, by forming the insertion opening 6 side of the sample container 100 into a truncated cone shape so as to taper, the tip of the sample container can be brought into linear circular contact with the tapered portion toward the elemental analyzer Z4 at the back side of the furnace body Z31 as shown in FIG. 8(c) to form a seal SL. That is, even if there is a small gap between the cylindrical portion of the cylindrical side wall 1 and the cylindrical portion of the furnace body Z31, allowing oxygen, which is a combustion gas, to pass through, the amount of leakage to the elemental analyzer Z4 side can be reduced by the seal SL formed between the tip of the sample container 100 and the tapered portion. Therefore, the amount of oxygen used as a combustion gas can be reduced, and the efficiency of supplying oxygen from the vent 4 to the sample W can be improved. Therefore, the combustion efficiency of the sample W can be increased compared to the conventional method.

[0061] As shown in Fig. 9, the sample container 100 may be provided with a metal plating GL such as gold plating or nickel plating in order to prevent the attachment of the element to be analyzed, which may cause contamination. Specifically, as shown in Fig. 9(a), the metal plating GL may be provided only on the outer peripheral surface of the cylindrical side wall 1, or as shown in Fig. 9(b), the metal plating GL may be provided only on the inner peripheral surface of the cylindrical side wall. Also, as shown in Fig. 9(c), the metal plating GL may be provided on both the outer peripheral surface and the inner peripheral surface of the cylindrical side wall 1. In this way, for example, carbon dioxide (CO) containing carbon (C), which is the element to be analyzed, can be easily removed. 2 ) from adhering to the surface of the sample container 100, and CO 2 This prevents the metal plating from being mixed in as a contaminant into the sample W.2 In addition, the cylindrical side wall 1 is the part having the largest surface area in the sample container 100, and therefore, the other parts such as the end faces can be sufficiently plated with metal to prevent CO 2 However, metal plating may be applied to all parts.

[0062] In order to prevent contamination during elemental analysis without applying a metal plating GL to the sample container 100, the position of the sample container 100 in the furnace body Z31 may be changed stepwise during heating as shown in Fig. 10. Specifically, the sample container 100 is initially placed at the inlet side of the furnace body Z31, where the temperature is lower than the center and where the sample W does not burn. In this first stage of preheating, the CO 2 etc. are desorbed, and a small amount of CO 2 is detected in elemental analyzer Z4. 2 When no more CO is detected or when heating of the sample container 100 at the inlet side for a predetermined time is completed, the sample container 100 is pushed into the center of the furnace body Z31. In this second stage, main heating is started at the center where the temperature is the highest, and the sample W starts to burn. In this state, CO, which may cause contamination, is not present in the sample container 100. 2 As shown in the graph, a large amount of CO was detected by the elemental analyzer Z4. 2 is the component gas (CO 2 ) can be used. By heating the sample container 100 in stages in this manner, contamination during elemental analysis can be reduced.

[0063] In the above embodiment, the sample container is made of quartz glass, but it may be made of other materials. However, the manufacturing cost and the CO generated in the blank measurement are increased. 2Considering the small amount of CO, it is preferable to form the sample container from quartz glass. Figure 11 shows the results of a blank measurement using single crystal silicon, alumina, the sample container of the above embodiment, and when no sample container was present in the furnace. When single crystal silicon and alumina were used, a larger amount of CO was emitted than when the sample container was made from quartz glass. 2 It can be seen that occurs in the blank measurement.

[0064] In the above embodiment, the sample container is cylindrical, but the cross-sectional shape may be, for example, a polygonal cylinder. The inner shape of the heating furnace and the outer diameter shape of the sample container are not limited to being the same, and a gap may be formed between the inside of the heating furnace and the outer surface of the sample container.

[0065] In the above embodiment, the end surface is formed with a hook portion, but a ring-shaped member or the like to which the hook portion of the rod can be hooked may be provided separately on one end side of the sample container. In other words, a part of the rod may be hooked on the hook portion without passing through the air hole.

[0066] The intrusion prevention member is not limited to a cylindrical shape, and may have other shapes, such as a plate-like member that separates the inside of the sample container and has a hole formed in part thereof through which the combustion gas can pass.

[0067] Furthermore, the configurations of the supply unit and the stocker unit are not limited to those shown in the above embodiment, but may be selected in various ways depending on the surrounding structure.

[0068] In addition, various modifications and combinations of the embodiments may be made as long as they do not go against the spirit of the present invention. [Industrial Applicability]

[0069] The present invention provides a sample container that improves analytical accuracy by removing elements adhering to the sample container and causing contamination prior to the generation of component gases.

Claims

1. A sample container used in an elemental analyzer that heats a sample and extracts and analyzes component gases, the sample container being inserted into a heating furnace of the elemental analyzer while containing the sample, The sample container comprises: A cylindrical side wall having a generally hollow cylindrical shape; The sample holder includes at least a pressure surface that is pressed by a rod when the sample holder is inserted into the heating furnace, and an air hole through which gas passes when the sample is heated. The pressure surface is provided at one end of the cylindrical side wall. a hook portion provided at the one end of the cylindrical side wall, on which a rod is hooked when the rod is removed from the heating furnace; A sample container characterized in that the hooked portion is an inner surface of the end face of the sample container.

2. 2. The sample container of claim 1, wherein the vent hole is sized to allow a portion of the rod to pass therethrough.

3. The heating furnace includes a furnace body having a generally hollow cylindrical shape and a predetermined inner diameter dimension, 3. A sample container according to claim 1, wherein said tubular side wall is generally hollow cylindrical in shape and has an outer dimension substantially equal to an inner diameter of said furnace body.

4. a sample insertion port for inserting the sample into the sample container is opened at the other end of the cylindrical side wall; 4. A sample container according to claim 1, wherein the inner diameter of said sample insertion port is larger than the inner diameter of said air hole.

5. A sample container as described in any one of claims 1 to 4, further comprising an intrusion prevention member provided on the one end side within the cylindrical side wall to prevent a rod inserted through the air hole from intruding beyond a predetermined position toward the other end side of the cylindrical side wall.

6. 6. A sample container according to claim 1, wherein at least an outer peripheral surface or an inner peripheral surface of said cylindrical side wall is metal plated.

7. 7. A sample container according to claim 1, wherein at least said cylindrical side wall is made of quartz glass.

8. A sample container according to any one of claims 1 to 7, An elemental analysis apparatus comprising the heating furnace, the heating furnace having a cylindrical furnace body having at least a portion of an inner diameter dimension that is approximately equal to the outer radial diameter dimension of at least a portion of the cylindrical side wall of the sample container.

9. Further comprising a gas analyzer for analyzing the extracted component gases, A narrowed portion is formed on the gas analyzer side of the furnace body, the narrowed portion being tapered toward the gas analyzer side, 9. An elemental analyzer according to claim 8, wherein an outer peripheral surface of said cylindrical side wall of said sample container opposite said end surface portion is tapered.

Citation Information

Patent Citations

  • Quartz boat

    CN207662754U

  • Sample automation loader

    JP1994273288A

  • Cable Housing System

    US20130091976A1