JPH0716141U - Sample preparation container for X-ray fluorescence analysis - Google Patents

Abstract

(57) [Abstract] [Purpose] Fluorescent X-ray analysis that does not cause cracks or collapse in the fluorescent X-ray analyzer, has a smooth and flat measurement surface, and can obtain highly accurate analysis results. A container capable of preparing a sample for use is provided. [Structure] An opening 3 is provided in a bottom surface 2A of an aluminum cup 2. [Effect] Since it is a bottomed container, it is possible to apply a sufficient pressing force during pressure molding, and it is possible to prepare an analytical sample that is excellent in shape retention and does not fall off during measurement. . Since the bottom surface has an opening, this opening functions as an air vent during pressure molding, and the air in the powder sample is smoothly extracted through this opening to perform sufficient air removal. be able to. It is possible to prepare an analytical sample that has almost no air bubbles, and therefore is free from the risk of cracking during measurement. Highly accurate analysis results can be obtained.

Description

[Detailed description of the device]

[0001]

[Industrial applications]

 The present invention relates to a sample preparation container for fluorescent X-ray analysis, and more particularly to improvement of an aluminum container for preparing a sample for fluorescent X-ray analysis by pressure molding a powder sample.

[0002]

[Prior art]

 When molding powder samples of dielectric materials such as barium titanate and strontium titanate as samples for fluorescent X-ray analysis by the pressure molding method, conventionally, as a pressure molding die, an aluminum ring, a chloride Vinyl rings or aluminum containers (hereinafter referred to as "aluminum cups") are used.

By the way, in order to obtain highly accurate analysis results by fluorescent X-ray analysis, it is necessary that the analysis sample does not have cracks or collapses during measurement, and the measurement surface of the analysis sample is smooth and flat. Needed.

[0004]

[Problems to be solved by the device]

 Among the above-mentioned conventional pressure-molding dies, the aluminum ring and the vinyl chloride ring have no bottom, so that the obtained sample for analysis has insufficient pressure and may fall off during measurement. Therefore, when using analytical samples obtained by pressure molding with these rings for measurement, we have taken measures to assist the bottom surface with paper or film.

On the other hand, in the case of an aluminum cup, since it has a bottom, sufficient pressure can be applied and there is no risk of the sample falling off. In addition to being covered by the air, the upper surface is also pressurized, so it is difficult to sufficiently extract the air mixed in the powder sample. Since the fluorescent X-ray analysis is performed in a vacuum, when using an analytical sample in which air is not sufficiently extracted and air bubbles are mixed, the air bubble portion in the sample in the fluorescent X-ray analyzer is used. There is a problem that cracks occur from the.

For this reason, conventionally, when pressure-molding a powder sample using an aluminum cup, pressure is not applied at once, but pressure is applied a little and then depressurized once, and then gradually applied. The work is done so that the air can be extracted as much as possible.

However, even if such a measure is taken, it is not possible to sufficiently extract air, and under the present circumstances, there is an analytical sample in which a crack is generated during measurement.

The present invention solves the above-mentioned conventional problems and provides a highly accurate analysis result with a smooth and flat measurement surface without the risk of cracks or collapse in the X-ray fluorescence analyzer. It is an object of the present invention to provide a container capable of preparing a sample for fluorescent X-ray analysis capable of performing the above.

[0009]

[Means for Solving the Problems]

 The sample preparation container for X-ray fluorescence analysis of the present invention is characterized by being made of a bottomed container made of aluminum and having an opening on the bottom surface.

[0010]

[Action]

 Since the sample preparation container for X-ray fluorescence analysis of the present invention has a bottomed container, it can apply a sufficient pressing force at the time of pressure forming, has excellent shape retention, and collapses during measurement. A fear-free analytical sample can be prepared.

Further, since the bottom surface is provided with an opening, this opening functions as an air vent hole during pressure molding, and air in the powder sample is smoothly extracted through this opening. Therefore, sufficient air can be removed. Therefore, it is possible to prepare a sample for analysis in which air bubbles are hardly mixed, and hence, cracks are not likely to occur during measurement.

[0012]

【Example】

 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

FIG. 1A is a plan view showing an embodiment of the sample preparation container for fluorescent X-ray analysis of the present invention, and FIG. 2B is a sectional view taken along the line BB of FIG. 1A. is there.

The sample preparation container 1 for X-ray fluorescence analysis of this embodiment is a container (aluminum cup) 2 having a bottom and provided with a plurality of (four in the figure) openings 3 on a bottom surface 2A thereof. is there.

Such an opening can be easily formed by making a hole in a predetermined portion of the bottom surface of the aluminum cup 2 using a drill or the like.

If the diameter of this opening is too large, for example, if it is about 3.5 mm, the portion of the obtained sample for analysis that is located at the opening is likely to collapse. On the other hand, if the pore size is too small, the air bleeding effect will be poor. Therefore, the pore size of the open pores is preferably about 1.5 to 2.5 mm, particularly about 2 mm.

The number of openings to be formed is preferably equal to a plurality of openings according to the properties of the sample powder, the size of the openings, etc. The number of openings is about 3 to 6, usually about 3 to 6. It is better to form four.

In order to prepare an analytical sample using such a fluorescent X-ray analytical sample preparation container 1, first, an aluminum cup 2 is uniformly filled with a powder sample for measurement, and then added according to a conventional method. Press forming. In this pressure molding, it is preferable that pressure is not applied all at once, and pressure is applied a little and then depressurized repeatedly to gradually apply pressure.

By such an operation, it is possible to sufficiently remove the air in the powder to obtain a high-precision analytical sample having a smooth and flat measurement surface without cracks or shavings.

When the aluminum cup is pressed, the vicinity of the center of the bottom surface rises, so it is preferable to perform the following operations in advance before subjecting to pressure molding. That is, first, in advance boost the bottom by applying a pressure of about 53~66t / cm ² in an aluminum cup, then, 164~178t / cm ² pressure of about at slightly less columnar body than the inner diameter of the A Rumikappu Add to the bottom of the aluminum cup to make the bottom flat. By performing such an operation, it becomes possible to form a sample for analysis having a higher shape accuracy. Hereinafter, the present invention will be described in more detail with reference to specific examples.

Embodiment 1 As shown in FIGS. 1A and 1B, an opening 3 having a diameter of 2 mm is formed in a bottom surface 2 A of an aluminum cup 2 having an outer diameter of 44 mm, an inner diameter of 40 mm (thickness of 2 mm) and a height of 10 mm. A strontium titanate powder, which is a dielectric material, was pressure-molded by using one formed in the center of the bottom surface and three formed around it at equal intervals to prepare a sample for analysis.

When the aluminum cup was pressed, the vicinity of the center of the bottom surface swelled, so the following treatment was performed.

First, a pressure of about 59 t / cm ² is applied to the aluminum cup to raise the bottom surface. Next, using a stainless steel cylinder having a diameter of 39 mm and a height of 30 mm, a pressure of about 178 t / cm ² was applied to the bottom surface to flatten the bottom surface. Next, 6.0 g of a strontium titanate sample was uniformly placed in the aluminum cup 2. The aluminum cup is sandwiched between dies and pressed to 59 t / cm ² with a pressure molding machine. Thereafter, the operation of temporarily lowering the pressure every 20 t / cm ² was repeated, and finally the pressure was increased to 178 t / cm ² for molding.

As a result, the air in the powder sample can be sufficiently extracted at the time of pressure molding, and the fluorescent X-ray analysis was performed using the obtained analysis sample. There was no risk of cracks on the sample surface even in a vacuum state, there was no risk of the sample falling off, the measurement surface was kept smooth and flat, and analysis could be performed with high analysis accuracy.

[0025]

[Effect of device]

 As described in detail above, according to the sample preparation container for X-ray fluorescence analysis of the present invention, there is no risk of cracks or collapse in the X-ray fluorescence analyzer, and the measurement surface is smooth and flat. An analytical sample that can be maintained at a low temperature can be easily prepared. Therefore, according to the analytical sample prepared by the sample preparation container for fluorescent X-ray analysis of the present invention, highly accurate analytical results can be obtained, and its industrial utility is extremely large.

[Submission date] September 8, 1993

[Procedure Amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0020

[Correction method] Change

[Correction content]

When the aluminum cup is pressed, the vicinity of the center of the bottom surface rises, so it is preferable to perform the following operations in advance before subjecting to pressure molding. That is, first, a pressure of about 590 to 660 kg / cm ² is applied to the aluminum cup to raise the bottom surface, and then a columnar body slightly smaller than the inner diameter of the aluminum cup has a pressure of about 1600 to 1800 kg / cm ^2. Add to the bottom of the aluminum cup to make the bottom flat. By performing such an operation, it becomes possible to form a sample for analysis with a higher shape accuracy. Hereinafter, the present invention will be described in more detail with reference to specific examples.

[Procedure Amendment 2]

[Document name to be amended] Statement

[Name of item to be corrected] 0023

[Correction method] Change

[Correction content]

First, the aluminum cup590 kg/ Cm² Apply pressure to raise the bottom. Next, using a stainless steel cylinder with a diameter of 39 mm and a height of 30 mm, 1800 kg / Cm² Was applied to the bottom surface to flatten the bottom surface. Next, 6.0 g of a strontium titanate sample was uniformly placed in the aluminum cup 2. Sandwich the aluminum cup with a die and use a pressure molding machine.590 kg/ Cm² Pressurize until After that,20 0 kg / Cm² Repeatedly lowering the pressure each time it increases, and finally18 00 kg / Cm² Molded by pressurizing to.

[Brief description of drawings]

FIG. 1 (a) is a plan view showing an embodiment of a sample preparation container for fluorescent X-ray analysis of the present invention, and FIG. 1 (b) is FIG. 1 (a).
It is sectional drawing which follows the BB line of FIG.

[Explanation of symbols]

 1 Sample preparation container for X-ray fluorescence analysis 2 Aluminum cup 3 Open hole

Claims (1)

[Scope of utility model registration request] 1. A sample preparation container for X-ray fluorescence analysis, which is made of an aluminum bottomed container and has an opening on the bottom surface.