JP2012058133A - Preparation instrument of sample for x-ray fluorescence analysis - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a preparation instrument of a sample for X-ray fluorescence analysis, having successful analysis sensitivity and less variation in analysis results, and allowing to easily obtain a solid sample suitable to be used in the X-ray fluorescence analysis.SOLUTION: The preparation instrument of the sample for the X-ray fluorescence analysis includes: a sample molding jig 10 having a metal frame 12 in which a sample raw material storage hole 11 is formed, a metal frame storage board 15 on which a metal frame storage hole 14 is formed, a base 13 for mounting the metal frame storage board 15 thereon, and a pressure board 16 arranged at a position opposite to the metal frame storage board 15 so as to sandwich the metal frame 12 stored in the metal frame storage board 15 to press the metal frame 12; and an overflow removal jig 20 having a base 21 for mounting the metal frame storage board 15 thereon including the metal frame 12, a holding member 22 arranged at a position opposite to the base 21 to hold the metal frame storage board 15 mounted on the base 21, and a lever 24 in which sample extrusion means 23 for extruding a molded solid sample from the metal frame storage board 15 held at the base 21 by the holding member 22 is formed.

Description

  The present invention relates to a sample preparation instrument for fluorescent X-ray analysis suitable for preparing a solid sample used for fluorescent X-ray analysis.

  In the preparation of a sample for fluorescent X-ray analysis, that is, a sample made of a solid used for fluorescent X-ray analysis (hereinafter referred to as a solid sample), a sample raw material that is a raw material of the solid sample is put into a metal frame, and a pressurizing apparatus Thus, there is known a production method for producing a solid sample by applying pressure to a metal frame containing a sample raw material and molding it into a predetermined size and shape.

  In such a production method, a plurality of solid samples are produced at the same time depending on the capacity of the pressure device. In addition, the solid sample used for fluorescent X-ray analysis is designed to increase the density of the solid sample and increase the density of the solid sample for the purpose of increasing the analytical sensitivity in the fluorescent X-ray analysis and making the analysis results difficult to vary. It is desirable to have a smooth surface.

JP 2006-71608 A JP 2006-242600 A JP-A-57-14746

  In order to increase the density of the solid sample and make the surface smooth, the sample material is made to overflow (overflow) from the metal frame when pressure is applied by a pressurizing device.

  At this time, the sample material overflows around the metal frame to form an overflow portion. The solid sample with the overflow portion attached cannot satisfy the standard of the fluorescent X-ray analyzer and cannot perform analysis, so the overflow portion must be removed.

  However, the removal of the overflow portion is performed manually so as to maintain the smoothness of the surface of the solid sample, so that the solid sample becomes dirty during the operation or foreign matter adheres to the solid sample (contamination). ) And the like may occur, and the analysis sensitivity may decrease.

  SUMMARY OF THE INVENTION An object of the present invention is to provide a sample preparation instrument for fluorescent X-ray analysis that has a good analytical sensitivity, has little variation in analysis results, and can easily obtain a solid sample suitable for use in fluorescent X-ray analysis. Is to provide.

  The present invention devised to achieve this object is a sample preparation instrument for fluorescent X-ray analysis for forming a solid sample used for fluorescent X-ray analysis by molding a sample raw material into a predetermined size and shape. A metal frame in which a sample material accommodation hole for accommodating a sample material is formed, a metal frame accommodation plate in which a metal frame accommodation hole for accommodating the metal frame is formed, and the metal frame accommodation plate And a pressure plate for pressurizing the metal frame disposed at a position facing the metal frame accommodation plate so as to sandwich the metal frame accommodated in the metal frame accommodation plate. , A base for placing the metal frame receiving plate including the metal frame taken out from the sample molding jig, and a base that is disposed at a position facing the base. A holding member for holding the metal frame housing plate including the mounted metal frame; An overflow removing jig having a lever formed with a sample pushing means for pushing out a solid sample molded from the metal frame housing plate including the metal frame held on the base by the holding member. It is a sample preparation instrument for fluorescent X-ray analysis.

  The press platen is preferably processed with a fluororesin on the surface in contact with the metal frame.

  A concave groove is formed on the metal frame housing plate at a position facing the base and facing the position where the metal frame housing hole is formed. It is preferable that a convex protrusion that fits into the groove formed on the metal frame housing plate is formed.

  The holding member may be formed with a guide hole so that the sample pushing means is guided to the metal frame when the lever is moved toward the holding member.

  According to the present invention, there is provided a sample preparation instrument for fluorescent X-ray analysis that has a good analytical sensitivity, has little variation in analysis results, and can easily obtain a solid sample suitable for use in fluorescent X-ray analysis. can do.

It is a perspective view which shows the sample shaping | molding jig of the sample preparation instrument for fluorescent X-ray analysis which concerns on this invention. It is a perspective view which shows the overflow removal jig | tool of the sample preparation instrument for a fluorescent X-ray analysis which concerns on this invention. It is a figure explaining the preparation method of the sample preparation for fluorescent X-ray analysis using the sample preparation instrument for fluorescent X-ray analysis which concerns on this invention.

  Preferred embodiments of the present invention will be described below with reference to the accompanying drawings.

  FIG. 1 is a perspective view showing a sample molding jig of a sample preparation instrument for fluorescent X-ray analysis according to a preferred embodiment of the present invention, and FIG. 2 is a perspective view showing the overflow removing jig.

  The sample preparation instrument for fluorescent X-ray analysis according to the present embodiment is for preparing a solid sample used for fluorescent X-ray analysis by molding a sample raw material into a predetermined size and shape. It consists of a jig 10 and an overflow removal jig 20.

[Configuration of sample molding jig]
As shown in FIG. 1, the sample molding jig 10 is formed with a metal frame 12 in which a sample raw material accommodation hole 11 for accommodating a sample raw material and a metal frame accommodation hole 14 for accommodating the metal frame 12 are formed. The position facing the metal frame accommodating plate 15 so as to sandwich the metal frame 12 accommodated in the metal frame accommodating plate 15, the base 13 for placing the metal frame accommodating plate 15, and the metal frame 12 accommodated in the metal frame accommodating plate 15. And a pressurizing plate 16 for pressurizing the metal frame 12.

  The sample material accommodation hole 11 of the metal frame 12 is formed so that the inner diameter thereof has a size and a shape that satisfy the standard of the fluorescent X-ray analyzer. The shape satisfying the standard indicates, for example, a cylindrical shape or a cubic shape.

  A concave groove 17 is formed on the metal frame housing plate 15 at a position facing the base 13 and a position facing the position where the metal frame housing hole 14 is formed. On the other hand, the base 13 is formed with a convex protrusion 18 that fits into the groove 17 formed in the metal frame housing plate 15. By fitting the grooves 17 and the protrusions 18, the metal frame housing plate 15 and the base 13 are fitted and fixed. In addition, as for these groove | channels 17 and the protrusions 18, it is desirable that each surface is processed with the fluororesin. This is because the metal frame housing plate 15 can be easily removed from the base 13 without stress after being pressurized by the pressure platen 16.

  Further, the metal frame housing plate 15 is formed with a smooth surface in contact with the pressure plate 16, and a plurality of metal frame housing holes 14 for housing the metal frame 12 are formed on the smooth surface. Yes. The metal frame accommodation hole 14 has a communication hole (not shown) having an inner diameter that is the same as or slightly larger than the sample raw material accommodation hole 11 formed in the metal frame 12 and communicates with the groove 17. . This communication hole is used to take out a solid sample processed from the metal frame 12 (a solid sample from which the overflow portion has been removed) when processing the solid sample formed by pressurization with an overflow removal jig 20 described later. It becomes a hole.

  The pressure plate 16 is composed of a low adhesion surface 19 whose surface on the metal frame 12 side (surface in contact with the metal frame 12) is subjected to low adhesion processing. This is to prevent the sample material from sticking to the pressure plate 16 when the sample material is pressurized. The low adhesion surface 19 is preferably low adhesion processed with a fluororesin excellent in low friction, heat resistance and chemical resistance.

[Configuration of overflow removal jig]
As shown in FIG. 2, the overflow removing jig 20 has a base 21 for placing the metal frame receiving plate 15 including the metal frame 12 taken out from the sample molding jig 10, and a position facing the base 21. A holding member 22 for holding the metal frame housing plate 15 including the metal frame 12 placed and placed on the base 21, and a metal frame housing plate 15 including the metal frame 12 held on the base 21 by the holding member 22. And a lever 24 formed with a sample extrusion means 23 for extruding a solid sample molded from the.

  The base 21 and the lever 24 are connected via a shaft portion 25, and are configured to be rotatable with respect to the shaft portion 25 as a boundary. On the base 21, a mounting portion 26 for mounting the metal frame accommodation plate 15 including the metal frame 12 is formed.

  The holding member 22 holds the metal frame housing plate 15 including the metal frame 12 after placing the metal frame housing plate 15 including the metal frame 12 on the mounting portion 26 on the base 21. In addition to this, when the holding member 22 is moved so as to close the lever 24 in the direction of the metal frame housing plate 15 including the held metal frame 12, the inside of the metal frame 12 is pressed by the sample pushing means 23. In order to separate the overflow portion from the solid sample formed on the metal frame housing plate 15, the overflow portion attached to the periphery of the metal frame 12 on the metal frame housing plate 15 is also a member that holds the metal frame housing plate 15.

  The holding member 22 is guided so that the sample pushing means 23 formed on the lever 24 is guided to the metal frame 12 on the metal frame housing plate 15 when the lever 24 is moved to the holding member 22 side. A hole 27 is formed on the metal frame 12. By this guide hole 27, the sample pushing means 23 is guided on the sample material accommodation hole 11 of the metal frame 12 in accordance with the movement of the lever 24, and is further moved to the metal frame accommodation plate 15 side so as to close the lever 24. The solid sample formed inside the metal frame 12 is extruded. The extruded solid sample is taken out of the overflow removing jig 20 from the groove 17 portion of the metal frame housing plate 15 through a take-out hole (communication hole) formed in the metal frame housing plate 15.

[Method for preparing a solid sample using a sample preparation instrument for fluorescent X-ray analysis]
A method of preparing a solid sample using the sample preparation instrument for fluorescent X-ray analysis will be described below with reference to FIG.

  First, as shown in FIG. 3A, the sample lower surface of the base 13 (the surface on which the metal frame housing plate 15 contacts) is smoothed to prevent the sample material from sticking when the sample material is pressure-molded. The groove 17 of the metal frame housing plate 15 is fitted into the protrusion 18 provided for the purpose.

  Next, as shown in FIG. 3B, the metal frame 12 is installed and accommodated in the metal frame accommodation hole 14 of the metal frame accommodation plate 15 provided to accommodate the metal frame 12, and the sample raw material is subjected to fluorescent X-ray analysis. A sample raw material is put in and stored in a sample raw material storage hole 11 for molding into a shape that satisfies the specifications of the apparatus.

  Then, as shown in FIG. 3 (c), the pressure plate 16 is placed on the upper part of the metal frame 12, the sample upper surface (the surface with which the metal frame 12 is in contact) is smoothed, and the sample material is subjected to pressure molding. It is installed with the low adhesion surface 19 provided in order to prevent the adhesion.

  Thereafter, when the metal frame 12 is pressurized from above the metal frame 12 with the pressure plate 16, a solid sample is formed in the sample material accommodation hole 11 and leaks from the sample material accommodation hole 11 to the upper surface of the metal frame accommodation plate 15. An overflow portion is formed by the sample material that has come out (overflowed).

  Next, as shown in FIG. 3 (d), the metal frame receiving plate 15 is slid horizontally from the base 13 and removed.

  Thereafter, as shown in FIG. 3 (e), the removed metal frame accommodation plate 15 is placed on a placement portion 26 for placing the metal frame accommodation plate 15 formed on the base 21 of the overflow removing jig 20. Put.

  After placing the metal frame housing plate 15, as shown in FIG. 3 (f), the overflow portion is moved between the metal frame housing plate 15 and the lever 24 by tilting the lever 24 toward the metal frame housing plate 15. A holding member 22 provided above the metal frame 12 for holding holds the overflow portion on the metal frame housing plate 15, and the sample pushing means 23 moves the solid sample formed in the sample raw material housing hole 11 upward. Push down from.

  As a result, the solid sample from which the overflow portion has been removed is taken out from a hole formed between the metal frame housing plate 15 and the base 21 by the groove 17 of the metal frame housing plate 15.

  As described above, according to the sample preparation instrument for fluorescent X-ray analysis according to the present embodiment, a solid sample used for fluorescent X-ray analysis is prepared by molding a sample raw material into a predetermined size and shape. A sample preparation tool for fluorescent X-ray analysis for a metal frame in which a sample material accommodation hole for accommodating a sample material is formed and a gold frame in which a metal frame accommodation hole for accommodating the metal frame is formed A frame housing plate, a base for mounting the metal frame housing plate, and a position facing the metal frame housing plate so as to sandwich the metal frame housed in the metal frame housing plate; A sample molding jig having a pressure plate for pressurizing the metal frame, a base for placing the metal frame receiving plate including the metal frame taken out from the sample molding jig, and the base The said metal frame accommodation containing the said metal frame arrange | positioned in the position which opposes, and was mounted in the said base A lever formed with a sample pushing means for extruding a solid sample molded from the metal frame housing plate including the metal frame held on the base by the holding member. By providing the overflow removing jig, the overflow portion can be removed without manual operation so as to maintain the smoothness of the surface of the solid sample when the overflow portion is removed. As a result, it is possible to prevent problems such as contamination of the solid sample during work and foreign matter adhering to the solid sample (contamination).

  In addition, in the conventional method of producing a solid sample by applying pressure to a sample material with a pressure device, the sample material is placed on the pressure plate surface of the pressure device depending on the properties of the sample material. It may stick. In such a case, since it is necessary to extract the sample raw material closely attached to the pressure plate surface from the pressure plate while paying attention to maintaining the smoothness of the surface, it takes time to work.

  On the other hand, in the sample preparation instrument for fluorescent X-ray analysis according to the present embodiment, the surface of the pressure plate 16 that is in contact with the metal frame 12 is processed with a fluororesin. It can be done in a short time.

  That is, according to the present invention, it is possible to easily obtain a solid sample having good analytical sensitivity and less variation in analysis results and suitable for use in fluorescent X-ray analysis.

  In this embodiment, the base 21 and the lever 24 are connected by the shaft portion 25. However, the base 21 and the lever 24 are not connected, and the lever 24 is opposed to the base 21. You may make it the pushing type pushed in so that surfaces may become parallel.

DESCRIPTION OF SYMBOLS 10 Sample shaping | molding jig | tool 11 Sample raw material accommodation hole 12 Metal frame 13 Base 14 Metal frame accommodation hole 15 Metal frame accommodation plate 16 Pressure board 17 Groove 18 Protrusion 19 Low adhesion surface 20 Overflow removal jig 21 Base 22 Holding member 23 Sample Extruding means 24 Lever 25 Shaft portion 26 Placement portion 27 Guide hole

Claims (4)

A sample preparation instrument for fluorescent X-ray analysis for forming a solid sample used for fluorescent X-ray analysis by molding a sample raw material into a predetermined size and shape,
A metal frame in which a sample material accommodation hole for accommodating a sample material, a metal frame accommodation plate in which a metal frame accommodation hole for accommodating the metal frame is formed, and the metal frame accommodation plate are placed. A sample having a base for pressurization and a pressurizing plate disposed at a position facing the metal frame housing plate so as to sandwich the metal frame housed in the metal frame housing plate and pressurizing the metal frame A molding jig,
Including a base for mounting the metal frame receiving plate including the metal frame taken out from the sample forming jig, and the metal frame placed on the base and disposed at a position facing the base. A holding member for holding the metal frame housing plate, and a sample extrusion means for extruding a solid sample molded from the metal frame housing plate including the metal frame held on the base by the holding member are formed. An overflow removal jig having a lever,
A sample preparation device for fluorescent X-ray analysis, comprising:   2. The sample preparation instrument for fluorescent X-ray analysis according to claim 1, wherein a surface of the pressure plate that is in contact with the metal frame is processed with a fluororesin. A concave groove is formed on the metal frame housing plate at a position facing the base and facing the position where the metal frame housing hole is formed,
The sample preparation instrument for fluorescent X-ray analysis according to claim 1 or 2, wherein a convex protrusion that fits into the groove formed in the metal frame housing plate is formed on the base.   The guide hole is formed in the said holding member so that the said sample extrusion means may be guided to the said metal frame when the said lever is moved to the said holding member side. The sample preparation instrument for fluorescent X-ray analysis as described.

Images