JP2013108778A - Sample preforming method and component quantification method using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample preforming method capable of improving analysis accuracy in component quantification by a fluorescent x-ray analysis method, and to provide a component quantification method using the preforming method.SOLUTION: In the sample preforming method to be used for the fluorescent x-ray analysis method after pressurization and principal forming, metal or alloy powder with 30 μm or less of average grain size D50 is filled in a mold and formed and the whole surface of a compact 5 to be irradiated with x-rays is pressurized by setting a pushing rate to 10 to 40%. When pressurizing the whole surface of the compact 5 to be irradiated with x-rays by setting the pushing rate to 10 to 40%, it is preferable to use a punch 4 for pressurizing the whole surface of the face irradiated with x-rays in the compact 5 and a guide 3 for guiding the punch 4, and it is also preferable to use oxide powder of rare earth-iron-boron group alloy as the metal or alloy powder.

Description

  The present invention relates to a method for preforming a sample used for fluorescent X-ray analysis and a component determination method using the same. More specifically, the present invention relates to a sample preforming method capable of improving analysis accuracy in component quantification by fluorescent X-ray analysis and a component quantification method using the same.

  There is a fluorescent X-ray analysis method as a method for quantifying the content of a substance. Component quantification by X-ray fluorescence analysis is performed, for example, by irradiating one surface of an analytical sample placed on a sample stage with X-rays and measuring fluorescent X-rays generated from the analytical sample at this time. This can be done using an analyzer.

When the target of component quantification is a metal or an alloy, the analytical sample can be prepared, for example, by the following procedure.
(A) The target metal or alloy is pulverized by a stamp mill or the like to obtain a powder having a predetermined particle size,
(B) Filling the mold with a powder to form a molded body, pre-molding (primary molding) into a sample by pressurizing the surface irradiated with X-rays with a flat spatula,
(C) The preformed sample is subjected to main molding (secondary molding) with a press machine to obtain a sample for analysis.

  In the preparation of the analytical sample by the procedures (a) to (c), a binder may be added to the pulverized metal or alloy powder as necessary. Further, after the pulverized metal or alloy powder is acid-dissolved, the acid-dissolved solution is adsorbed on the filter paper powder and fired to fill the mold as a powder containing the metal or alloy as an oxide.

  Various proposals have heretofore been made regarding component quantification by such X-ray fluorescence analysis, and for example, Patent Document 1 is available. In the component determination method proposed in Patent Document 1, an alloy having an active metal is pulverized into a powder of D50 = 10 to 40 μm, and then subjected to pressure molding (main molding) using a mold and a press machine for analysis. Sample for use. In addition, in patent document 1, it does not describe about the preforming of (b) among preparation of the analytical sample which consists of the procedure of said (a)-(c).

  In such a component determination method proposed in Patent Document 1, the sample is made from an alloy powder having a D50 of 10 to 40 μm by pulverization, so that ignition is not caused without causing deterioration in analysis accuracy and reproducibility. It can be prevented.

  However, using the analysis sample prepared by the procedure of (a) to (c) and the analysis sample prepared from the powder having the particle diameter proposed in Patent Document 1, components are quantified by fluorescent X-ray analysis. Even when samples for analysis are produced from the same metal or alloy powder by the same procedure, the analysis results vary for each analysis sample. For this reason, in component quantification by fluorescent X-ray analysis, it has been desired to improve the analysis accuracy by reducing the variation in the analysis results.

JP 2003-172714 A

  As described above, in the component quantification by the conventional fluorescent X-ray analysis method, the analysis result varies. Therefore, it has been desired to improve the analysis accuracy by reducing the variation of the analysis result. The present invention has been made in view of such a situation, and an object of the present invention is to provide a sample preforming method that can improve analysis accuracy in component quantification by fluorescent X-ray analysis and a component quantification method using the same. To do.

  The present inventors examined the reason why the analysis results vary in the component quantification by the conventional fluorescent X-ray analysis method. Here, in the preparation of the analysis sample according to the procedures (a) to (c), the surface on which the X-ray of the compact made of metal or alloy powder is irradiated in the preliminary molding in the procedure (b) is flattened. Apply pressure while leveling.

  Since the flat spatula used in the preforming is usually smaller in area than the surface irradiated with X-rays, the surface irradiated with X-rays is pressurized in a plurality of areas in several areas. Further, since pressurization with a flat spatula is usually performed manually, the force of pressurization changes each time. For this reason, the preformed sample varies in the particle density depending on the location on the surface layer portion of the X-ray irradiation surface.

  Furthermore, since pressurization with a pre-formed flat spatula is an operation based on the experience of the operator, the pressurizing force changes depending on the operator. From these, the preformed sample varies with the particle density of the surface layer portion of the X-ray irradiation surface changing for each sample.

  As a result, even in the analytical sample that is formed by pressurization with a press, the particle density in the surface layer portion of the surface irradiated with X-rays varies. As described above, the variation in the particle density in the surface layer portion of the surface irradiated with X-rays generated in the analytical sample may cause the analytical value to vary when the analytical sample is used for component determination by the fluorescent X-ray analysis method. The present inventors have found out. Here, the “surface layer portion” means a portion where information can be obtained in component quantification by fluorescent X-ray analysis, and is usually in a range of about 100 μm from the surface irradiated with X-rays.

  Therefore, as a result of conducting various tests and intensive studies, the present inventors have used a punch that pressurizes the entire surface to be irradiated with X-rays and a guide for guiding the punch, and a metal or alloy powder. It was found that the particle density in the surface layer portion of the surface irradiated with X-rays can be made uniform by pressurizing and pre-molding a molded body made of Further, the present inventors have found that the analysis accuracy can be improved by quantitatively determining the components by fluorescent X-ray analysis after the preformed sample is fully molded.

  The present invention has been completed on the basis of the above findings, and the gist of the present invention is the sample pre-forming method (1) to (3) below and the component quantification method of the sample (4) below.

(1) A method of pre-molding a sample to be used for fluorescent X-ray analysis after pressurizing and main-molding, filling a mold with metal or alloy powder having an average particle diameter D50 of 30 μm or less, and molding the mold, A pre-molding method for a sample, characterized in that the entire surface of the molded body that is irradiated with X-rays is pressed with an indentation rate calculated by the following formula (1) set to 10 to 40%.
P = 100 × (h1−h2) / h1 (1)
Here, the height of the compact before pressurization is h1 (mm), and the height of the compact after pressurization is h2 (mm).

(2) a punch that pressurizes the entire surface of the molded body that is irradiated with X-rays, and pressurizes the entire surface of the molded body that is irradiated with X-rays when the pressing rate is 10 to 40%. The method for preforming a sample as described in (1) above, wherein a guide for guiding the punch is used.

(3) The method for preforming a sample as described in (1) or (2) above, wherein an oxide powder of a rare earth-iron-boron alloy is used as the metal or alloy powder.

(4) A method for quantitatively determining components by fluorescent X-ray analysis after performing main molding by pressurizing a sample, and the preforming method according to any of (1) to (3) above as the sample A method for quantifying a component of a sample, characterized in that a sample preformed by the method is used.

  The preforming method of the present invention makes the particle density in the surface layer portion of the surface of the preformed sample irradiated with X-rays uniform by pressurizing the entire surface of the molded body irradiated with X-rays. Can do. If a sample having a uniform particle density in the surface layer portion of the surface irradiated with X-rays is formed in this manner, the particle density in the surface layer portion of the surface irradiated with X-rays becomes uniform in the molded sample for analysis. In addition, it is possible to improve analysis accuracy in component quantification by X-ray fluorescence analysis.

  Since the component quantification method of the present invention uses the preforming method of the present invention having the above-described effects, the analysis accuracy of component quantification can be improved.

It is a schematic diagram explaining the example of the preparation procedure of the sample by the preforming method of this invention, The figure (a) fills a type | mold with the powder and it is the molded object, The figure (b) inserts a punch in a guide Each state is shown.

  Hereinafter, the preforming method of the present invention and the component determination method using the same will be described with reference to the drawings.

  FIG. 1 is a schematic diagram for explaining an example of a sample preparation procedure according to the preforming method of the present invention. FIG. 1 (a) shows a state in which a mold is filled with powder, and FIG. 1 (b) shows a guide. Each shows a state in which a punch is inserted. The figure shows a work table 1, an annular sample ring 2 that forms a mold for molding together with the work table 1, a molded body 5 made of metal or alloy powder filled in the molding mold, and a molded body 5 2 shows a punch 4 for pressurizing and a guide 3 for guiding the punch 4.

  The preforming method of the present invention is a method of preforming a sample to be used for fluorescent X-ray analysis after press molding and filling with a metal or alloy powder having an average particle diameter D50 of 30 μm or less. Then, the entire surface of the surface 5a irradiated with X-rays of the molded body 5 is pressed with the indentation rate calculated by the equation (1) set to 10 to 40%.

  The reason why the average particle diameter D50 of the metal or alloy powder is defined as 30 μm or less is that when the average particle diameter D50 exceeds 30 μm, the proportion of particles having a large particle diameter increases, and the formability deteriorates in preforming and main forming. Therefore, the flatness of the surface irradiated with X-rays in the analysis sample is deteriorated. As a result, irregular reflection increases in component quantification by fluorescent X-ray analysis, and the analysis accuracy decreases. On the other hand, if the average particle diameter D50 is too small, some of the particles enter the gap between the punch and the guide when pre-molding using the punch and the guide, causing problems such as galling, and so on. It is preferable to do this.

  Here, in the present invention, the average particle size D50 means a particle size having a cumulative frequency of 50% in the volume-based particle size distribution, and the particle size distribution is determined using a measuring device by a laser diffraction scattering method.

  In the preforming method of the present invention, a metal or alloy powder having an average particle diameter D50 in the above range is filled into a mold and molded, and the entire surface 5a irradiated with X-rays of the molded body 5 has an indentation rate of 10 Pressurize to ~ 40%. In the conventional component quantification by the conventional fluorescent X-ray analysis method, as described above, preforming is performed manually using a flat spatula having a smaller area than the surface 5a irradiated with X-rays. The particle density varies depending on the location on the surface layer portion of the X-ray irradiation surface.

  On the other hand, in the preforming method of the present invention, the entire surface 5a of the molded body 5 to which X-rays are irradiated is pressurized. Thereby, since the whole surface 5a irradiated with X-rays of the molded body 5 is pressurized with the same force, the particle density in the surface layer portion of the surface irradiated with X-rays is uniform without changing depending on the location. Become. If the preformed sample is used as the main molding, the particle density in the surface layer portion of the surface irradiated with X-rays becomes uniform in the analytical sample thus molded, and analysis in component quantification by fluorescent X-ray analysis is performed. Accuracy can be improved.

  Moreover, when pressurizing the whole surface 5a to which the X-ray of the molded body 5 is irradiated, the indentation rate calculated by the equation (1) is set to 10 to 40%. The indentation rate P calculated by the above equation (1) is the amount of change in the height of the molded body before and after pressing (h1-h2, unit: mm), and the height of the molded body before pressing (h2, unit). : Mm) and expressed as a percentage.

  When the indentation rate is less than 10%, the effect of making the particle density of the surface layer portion uniform is almost not exhibited by pressurizing the entire surface of the molded body that is irradiated with X-rays. Variation occurs in the particle density of the surface layer portion of the surface to which the sample is irradiated with X-rays. For this reason, the particle density of the analysis sample thus formed varies and cracks occur. When cracks occur in the analysis sample, the analysis results greatly vary in component quantification by fluorescent X-ray analysis, and effective analysis results cannot be obtained.

  On the other hand, if the indentation rate exceeds 40%, the powder particles are biased toward the outer edge of the molded body, and the particle density in the surface layer portion of the surface irradiated with X-rays in the preformed sample varies. For this reason, the particle density of the analysis sample thus formed varies and cracks occur.

  As described above, the preforming method of the present invention pressurizes the entire surface of the molded body that is irradiated with X-rays, so that the particle density in the surface layer portion of the surface that is irradiated with X-rays in the preformed sample is uniform. Can be. If this molded body is formed, the analysis sample also has a uniform particle density in the surface layer portion of the surface irradiated with X-rays, and the analysis accuracy in component quantification by fluorescent X-ray analysis can be improved.

  The preforming method of the present invention can be applied by an operator if the indentation rate is controlled to a certain value within the above-mentioned range when pressing the entire surface of the molded body irradiated with X-rays. It is possible to prevent the conditions from changing, and it is possible to suppress variations in the particle density of the surface layer portion of the X-ray irradiation surface for each preformed sample. As a result, in the component quantification by the fluorescent X-ray analysis method, it is possible to reduce the variation in the measured value for each analytical sample and improve the analysis accuracy.

  In the preforming method of the present invention, when the entire surface of the molded body 5 irradiated with X-rays is pressed at a pressing rate of 10 to 40%, the entire surface 5a of the molded body 5 irradiated with X-rays. It is preferable to use a punch 4 for pressurizing and a guide 3 for guiding the punch 4. Below, it is an example of the process sequence by the preforming method of this invention, Comprising: The process sequence in the case of using the punch 4 and the guide 3 is demonstrated in detail, referring said FIG.

  As shown in FIG. 1A, a molding die is formed by the inner surface of the annular sample ring 2 and the planar upper surface of the work table 1. A guide 3 is placed on the sample ring 2 and a molding die is filled with a metal or alloy powder to form a disk-shaped molded body 5.

  Next, a cylindrical punch 4 is inserted into the hollow portion of the guide 3 as shown in FIG. When the punch 4 is moved (lowered) by the guide 3, the molded body 5 and the punch 4 come into contact with each other, and the punch 4 has a cross-sectional shape corresponding to the cavity (the cross-sectional shape of the mold) of the sample ring 2. The entire surface 5a of the molded body 5 irradiated with X-rays is pressurized by the punch 4. The punch 4 is further moved (lowered) and moved (lowered) until the indentation rate becomes 10 to 40%.

  Thus, by using the punch 4 that pressurizes the entire surface 5 a of the molded body 5 to which X-rays are irradiated and the guide 3 that guides the punch 4, the surface of the molded body 5 that is irradiated with X-rays. The entire surface of 5a can be easily and uniformly pressurized. Further, if the metal or alloy powder is filled in the mold for molding with the guide 3 placed on the sample ring 2, the metal or alloy powder can be prevented from being scattered.

As shown in the figure, when the disk-shaped molded body 5 is formed using the annular sample ring 2, the inner diameter D2 (mm) of the guide 3 is as follows with the outer diameter of the cylindrical punch 4 being D1 (mm). It is preferable to design so as to satisfy the formula (2). As a result, the punch 4 can be moved smoothly along the guide 3, and metal or alloy powder can be prevented from entering the gap between the guide 3 and the punch 4 during pressurization.
D1 + 0.01 ≦ D2 ≦ D1 + 0.05 (2)

Further, it is preferable that the outer diameter of the cylindrical punch 4 is D1 (mm) and the inner diameter of the sample ring 2 is D3 (mm) so that the following expression (3) is satisfied. This makes it possible to pressurize the entire surface 5a of the molded body that is irradiated with X-rays, and to prevent deterioration in workability and increase in manufacturing cost due to the enlargement of the punch 4 and the guide 3.
D3 ≦ D1 ≦ D3 + 0.01 (3)

  Since the punch 4 and the guide 3 pressurize metal or alloy powder, it is preferable to use high-strength steel or alloy. For example, stainless steel (SUS type) or carbon tool steel (SK type) can be adopted. It is more preferable to use a cemented carbide (for example, WC-Co type or WC-TiC-Co type).

  In the preforming method of the present invention, a binder may be added to metal or alloy powder and kneaded and then filled into a mold. As a result, it is possible to prevent a part of the pre-molded sample and the analytical sample obtained by molding the molded body from being pulverized by vibration or the like. As the binder, for example, stearic acid or a styrene-maleic acid copolymer can be used.

  In the preforming method of the present invention, the metal or alloy powder may be formed into an oxide and then filled into a mold. The oxide can be obtained, for example, by dissolving a metal or alloy powder with an acid, adsorbing the acid solution on a filter paper powder, and baking it.

  The metal or alloy is not particularly limited, and a pure metal, an alloy, or the like can be used as a powder. If the metal or alloy powder is a powder having high hardness (high Young's modulus) with little springback when pressed, the particle density in the surface layer portion of the surface irradiated with X-rays in the preformed sample according to the present invention The effect of making uniform becomes larger. For this reason, the preforming method of the present invention is suitable for preparing an analytical sample from an oxide powder of a rare earth-iron-boron alloy.

  The component quantification method of the present invention is a method of quantitatively determining components by fluorescent X-ray analysis after performing main molding by pressurizing a sample, wherein a sample preformed by the above-described preforming method of the present invention is used as a sample. It is characterized by using. As described above, since the sample preformed by the preforming method of the present invention has a uniform particle density in the surface layer portion of the surface irradiated with X-rays, the analysis sample thus formed is also irradiated with X-rays. The particle density is uniform in the surface layer portion of the surface. For this reason, the component quantification method of the present invention can improve analysis accuracy in component quantification by fluorescent X-ray analysis.

  In the component quantification method of the present invention, the main molding by pressurizing the sample can be performed by an apparatus such as a uniaxial press.

  In order to verify the effects of the preforming method of the present invention and the component determination method using the same, the following tests were conducted.

1. Component quantification test [test method]
In this test, a powder A made of an oxide of an alloy and an alloy powder B were prepared, and the preparation procedure of the powder A was as follows. A slab of a rare earth-iron-boron alloy cast by the strip casting method (Nd: 32.3% by mass and B: 1.0% by mass and the balance of Fe) is crushed with hydrogen and then sieved Classification was performed with a sieve having a mesh size of 0.5 mm. A mass of 4.2 g was sampled from the alloy powder under the sieve, dissolved in nitric acid (HNO ₃ ) by heating, and the dissolved liquid was adsorbed on the filter paper powder and then incinerated in the form of a heated steel plate. After the ashed product is pulverized by a stamp mill to form a powder, it is fired by heating in an electric furnace under certain conditions, and a powder having a mass of 4.5 g made of an oxide of a rare earth-iron-boron alloy. A was obtained.

  On the other hand, the preparation procedure of the powder B was as follows. The mixed raw material was heated and melted in a vacuum, and this molten metal was poured into a mold to obtain an alloy ingot. At this time, the mixed raw materials were blended so that the composition of the alloy ingot was Ti: 30% by mass and Ni: 70% by mass. The obtained alloy ingot was pulverized with a stamp mill and then classified with a sieve having a sieve mesh of 20 μm.

  About these powder A and B, the particle size distribution was measured using the measuring machine (Shimadzu Corporation make, SALD3000S) by the laser diffraction scattering method, and the average particle diameter D50 was 5 micrometers for powder A, and 10 micrometers for powder B.

  In the present invention example, after filling the mold with powder A or B according to the procedure described with reference to FIG. 1, the entire surface of the surface irradiated with X-rays is pressed. Was preformed by pressurizing to 19%. At this time, the outer diameter of the annular sample ring was 37.8 mm, the inner diameter was 31.0 mm, the outer diameter of the punch was 31.0 mm, and the inner diameter of the guide was 31.03 mm. Stainless steel (SUS316) was used for the punch and guide. This pre-molded sample was formed into a sample for analysis by main molding with a press machine, and the press machine was pressurized under a condition of 150 kN using a uniaxial press machine.

  In the conventional example, an annular sample ring is arranged on a work table having a flat upper surface, and a mold formed by the inner surface of the sample ring and the upper surface of the work table is filled with powder A or powder B to form a molded body. A surface (upper surface) irradiated with X-rays of this molded body was preliminarily molded by pressurizing while flattening with a flat spatula, and the preformed sample was subjected to main molding with a press machine to obtain a sample for analysis. The pre-formed flat spatula is 10 mm long and 10 mm wide to press the compact, and the press machine of this molding was pressurized using a uniaxial press machine at 150 kN.

  For the powder A, 5 samples for analysis were prepared for each of the present invention example and the conventional example, and the Nd component of the sample for analysis was quantified with a fluorescent X-ray analyzer (manufactured by Rigaku Corporation, Simulix 14). For powder B, five analytical samples were prepared for each of the present invention example and the conventional example, and the Ni component of each analytical sample was quantified using a fluorescent X-ray analyzer. Component quantification using a fluorescent X-ray analyzer was performed under the measurement conditions of a tube voltage of 50 kV, a tube current of 50 mA, and a measurement time of 40 seconds.

[Test results]
Table 1 shows the content (% by mass) of the Nd component quantified in each analytical sample using the powder A in the present invention example or the conventional example. Table 1 also shows the average value, standard deviation, and coefficient of variation (standard deviation / average value) of the content of the Nd component in the present invention example or the conventional example.
On the other hand, Table 2 shows the content (mass%) of the Ni component quantified in each analytical sample using the powder B in the present invention example or the conventional example. In addition, Table 2 also shows the average value, standard deviation, and coefficient of variation (standard deviation / average value) of the Ni component content in the present invention example or the conventional example.

From Table 1, the standard deviation of the content of the Nd component in the analytical sample using powder A was 0.04 in the conventional example, but 0.02 in the present invention example.
On the other hand, from Table 2, the standard deviation of the Ni component content in the analytical sample using powder B was 0.06 in the conventional example, and 0.03 in the present invention example.

  From these, it is clear that the analysis accuracy can be improved in the component quantification by the fluorescent X-ray analysis method by filling the alloy powder into the mold and molding it, and pressurizing the entire surface of the compact that is irradiated with X-rays. became.

2. Pre-molding test [test method]
In this test, the above-mentioned powder A or B was used as a molded body, and this molded body was pre-molded by pressurization according to the procedure described with reference to FIG. A sample for analysis was obtained by press-molding the preformed sample under a condition of 150 kN using a single-screw press and performing main molding.

  In this test, the indentation rate was changed from 8 to 48% when powder A was used and 6 to 48% when powder B was used when pre-molding the compact by pressing. At this time, sample rings, punches, and guides having the same dimensions and materials as those of the present invention example of “1.

In this test, the presence or absence of cracks was visually confirmed on the surface of the obtained analytical sample that was irradiated with X-rays. The meanings of the symbols in the crack evaluation column of Table 3 and Table 4 to be described later are as follows.
(Circle): It shows that the crack was not confirmed by the surface irradiated with the X-ray of the sample for analysis.
X: It shows that the crack was confirmed by the surface irradiated with the X-ray of the sample for analysis.

[Test results]
Table 3 shows the test number, classification, height of the molded body before pressing (h2) in the test using powder A, and the difference between the height of the molded body before pressing and the height of the molded body after pressing ( h1-h2), the indentation rate, and the results of crack evaluation of the molded sample for analysis are shown.
On the other hand, Table 4 shows the test number, classification, height of the compact before pressing (h2), the height of the compact before pressurization and the height of the compact after pressurization in the test using powder B. The difference (h1−h2), the indentation rate, and the result of crack evaluation of the molded sample for analysis are shown.

  From Table 3, when powder A is used, X of the analytical sample formed in this way was obtained by test numbers 3-1 having an indentation rate of less than 10% and test numbers 3-8 and 3-9 exceeding 40%. Cracks were confirmed on the surface irradiated with the line. On the other hand, in the test numbers 3-2 to 3-7 in which the indentation rate was 10 to 40%, no cracks were confirmed on the surface of the analytical sample that was subjected to X-ray irradiation.

  From Table 4, when powder B was used, X of the analytical sample formed in this way was obtained by test numbers 4-1 having an indentation rate of less than 10% and test numbers 4-8 and 4-9 exceeding 40%. Cracks were confirmed on the surface irradiated with the line. On the other hand, in the test numbers 4-2 to 4-7 in which the indentation rate was 10 to 40%, no cracks were confirmed on the surface of the analytical sample that was subjected to X-ray irradiation.

  From these, the whole surface of the molded body irradiated with X-rays is pressed with an indentation rate of 10 to 40%, so that the analytical sample thus formed does not crack, and as a result, fluorescent X-rays are obtained. It became clear that the analysis accuracy could be improved in the component quantification by the analytical method.

  The preforming method of the present invention makes the particle density in the surface layer portion of the surface of the preformed sample irradiated with X-rays uniform by pressurizing the entire surface of the molded body irradiated with X-rays. Can do. If a sample having a uniform particle density in the surface layer portion of the surface irradiated with X-rays is formed in this manner, the particle density in the surface layer portion of the surface irradiated with X-rays becomes uniform in the molded sample for analysis. In addition, it is possible to improve analysis accuracy in component quantification by X-ray fluorescence analysis. In addition, since the component quantification method of the present invention uses the preforming method of the present invention having the above-described effects, the analysis accuracy of component quantification can be improved.

  Therefore, if the preforming method of the present invention and the component determination method using the same are applied to the production of a rare earth-iron-boron alloy used as a raw material for a rare earth magnet, the quality of the rare earth-iron-boron alloy is greatly improved. Can contribute.

1: work table, 2: sample ring, 3: guide, 4: punch,
5: Molded body (sample), 5a: surface irradiated with X-rays, D1: outer diameter of punch,
D2: inner diameter of the guide, D3: inner diameter of the sample ring

Claims (4)

A method for pre-molding a sample to be used for fluorescent X-ray analysis after press molding and main molding,
A metal or alloy powder having an average particle diameter D50 of 30 μm or less is filled into a mold and molded, and the entire surface of the molded body that is irradiated with X-rays has an indentation rate calculated by the following formula (1) of 10 to 10 A method for preforming a sample, wherein the pressure is 40%.
P = 100 × (h1−h2) / h1 (1)
Here, the height of the compact before pressurization is h1 (mm), and the height of the compact after pressurization is h2 (mm).   A punch that pressurizes the entire surface of the molded body that is irradiated with X-rays and pressurizes the entire surface of the molded body that is irradiated with X-rays, and presses the punch. The method for preforming a sample according to claim 1, wherein a guide for guiding is used.   The method for preforming a sample according to claim 1 or 2, wherein an oxide powder of a rare earth-iron-boron alloy is used as the metal or alloy powder. A method for quantitatively determining a component by fluorescent X-ray analysis after main molding by pressurizing a sample,
A sample component quantification method using a sample preformed by the preforming method according to claim 1 as the sample.

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