JPH11344455A - X-ray fluorescence X-ray analysis method for sample mask, sample holder and slag - Google Patents

Abstract

(57) [Summary] [PROBLEMS] To directly perform X-ray fluorescence analysis on a solid sample piece,
Provided are a sample mask for X-ray fluorescence analysis, a sample holder, and a method of X-ray fluorescence analysis of slag, which can prevent a decrease in analysis accuracy due to irregularities on the sample surface. SOLUTION: This is a fluorescent X-ray analysis sample mask 2 having an opening 6 for irradiating primary X-rays and extracting characteristic X-rays, and surrounds the opening 6 on a surface of the sample mask 2 facing the sample. A sample mask provided with the projection 4, a sample holder using the sample mask, and a molten slag are adhered to the peripheral surface of a prismatic sampler or a plate-like sampler, quenched and solidified, and then peeled off. A slag X-ray fluorescence analysis method in which a simple analysis surface is brought into contact with the projection 4 of the sample mask 2 and X-ray fluorescence analysis is performed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample mask and a sample for X-ray fluorescence analysis, which are capable of preventing a decrease in analysis accuracy due to unevenness of the sample surface when directly performing X-ray fluorescence analysis on a solid sample piece. Regarding the holder. Furthermore, the present invention quickly analyzes slag that plays an important role in controlling the composition of steel and pig iron in the steel refining process and pig iron manufacturing process, and operates online based on the obtained analysis results. The present invention relates to a method for X-ray fluorescence analysis of slag which can provide the guidelines described in the above.

[0002]

2. Description of the Related Art Generally, glass bead fluorescent X-ray analysis, which can simultaneously analyze multiple elements with high accuracy, is used for slag analysis. This method uses a crushed slag of about 0.
In this method, 3-0.5 g is melted using about 5 g of a flux such as sodium borate, and a homogeneous glassy sample is prepared for X-ray fluorescence analysis.

[0003] In this method, the analysis accuracy is excellent because the sample is homogenized by melting and is diluted with a flux, so that the influence of coexisting elements in the fluorescent X-ray analysis is small. I have. However, the operations of grinding, weighing, and melting usually require at least 30 minutes, which is problematic in terms of analysis time.

On the other hand, when quickness and simplicity are required, the briquetting method may be used. In this method, after slag is crushed, it is subjected to pressure molding directly or in a container, and the obtained molded body, ie, briquette, is subjected to X-ray fluorescence analysis. This method has a shorter analysis time than the glass bead method because there is no work of weighing and melting, but it requires at least 25 to 30 minutes to wash the container together at the time of pulverization.

Further, even if the above-mentioned glass bead method or briquette method is set up as an efficient automatic system, it is difficult to reduce the analysis time to 20 minutes or less (Kokura et al., NKK Technical Report, No. 128, p. 49 (1989)). For this reason, Japanese Patent Application Laid-Open No. 9-166589 discloses a method of performing X-ray fluorescence analysis of a collected sample itself for the purpose of shortening the analysis time.

[0006] In the above method, a sampler having a flat surface larger than a circle having a diameter of 10 mm is inserted into a molten slag layer of molten steel, the slag is attached to the flat surface, the sampler is pulled up from the slag layer, and the solidified slag is separated. Then, the slag adhered to the flat surface is used to irradiate X-rays on the surface opposite to the side in contact with the sampler to perform fluorescent X-ray analysis.

However, in this method, in the process of cooling and solidifying the slag, a component distribution occurs in the thickness direction of the attached slag due to the difference in the solidification temperature of the oxide in the slag. In particular, the effect is remarkable on the surface of the slag sample which solidifies last, that is, the sample surface opposite to the side in contact with the sampler. Therefore, when this surface is analyzed, the analysis value is significantly different from the average composition of the slag.

In general, in the steel refining process and the pig iron manufacturing process, the molten metal level fluctuates during operation, and slag is mixed with steel or pig iron, and the viscosity of the slag depends on the type of steel or time-series operation conditions. , The flat measurement surface cannot always be obtained by this method, and the analysis accuracy is lowered. Due to such a problem, the technology disclosed in the above publication is not practical, and slag analysis is generally performed by the above-described glass bead method or briquette method.

As described above, the analysis of slag is carried out by the glass bead method or the fluorescent X-ray analysis method using the briquette method. Both methods require time for sample preparation, and are at least 25 to 30 minutes. Because of the required analytical methods, it is difficult to obtain analytical results during steel refining. Also, the method of directly analyzing the non-contact surface of the cooled and solidified slag sample with the sampler cannot obtain sufficient accuracy for the above-described reason.

However, in the steel refining process, changes in the composition of slag have a great effect on the control of the composition of the steel itself. Therefore, if the composition of the slag can be known during refining, it can greatly contribute to the control of operating conditions. . Also, in the pig iron production process, if it is possible to analyze the composition of slag in a short time, it is possible to control the blast furnace more quickly, and it can be expected to contribute to stabilization of operation.

From the above, the present inventors have solved the above-mentioned problems of the prior art, and analyzed slag quickly in the steel refining process and the pig iron manufacturing process, and based on the obtained analysis results. A method and apparatus for preparing a slag sample for X-ray fluorescence analysis capable of accurately and easily analyzing the slag composition within a few minutes at a manufacturing site so as to provide an operation guideline online (Japanese Patent Application No. 10-57460).

In this technique, a prismatic or rod-shaped sampler is immersed in a molten slag, the molten slag is attached to the peripheral surface of the sampler, the sampler is pulled up, the solidified slag is separated, and the slag is mixed with the sampler. This method enables rapid analysis of slag by fluorescent X-ray analysis of the contact surface. According to this method and apparatus, sample preparation such as pulverization is not required, and slag composition is reduced in a few minutes with almost no influence of segregation. Can be analyzed.

However, when the above technique is applied, there is room for improvement in a method of setting a slag specimen to a specimen holder for X-ray fluorescence analysis. Typically,
In the fluorescent X-ray analysis method, the sample is set by contacting the sample with a mask portion of a smooth sample holder. The slag sample piece collected by the prism-shaped sampler has a smooth analytical surface, but the molten slag is adhered and solidified on the peripheral surface of the prism, and the peeled amorphous flakes are used. A projection may be formed on the analysis surface side of the slag sample piece due to the corner portion.

When the projections are formed, when the analysis surface is brought into contact with the above-mentioned smooth sample mask, the projections come into contact with the mask, and the surface to be analyzed is shifted from a normal position. To cause an analysis error. On the other hand, in the operation of the iron and steel refining process and the pig iron manufacturing process, quick analysis is required, so that it is not preferable to perform operations such as polishing to remove the protrusions.

When a wavelength-dispersive X-ray fluorescence spectrometer is used, information from the analysis surface is averaged, and the sample is rotated so that even if the analysis surface has a small amount of irregularities, it is not affected by the unevenness. It is essential to perform analysis by using a sample, but simply placing an irregularly shaped slag sample with many protrusions on the sample holder only contacts the holder and the sample at a point and may move during rotation. .

If the sample moves, not only will an analysis value error occur, but also a part of the sample may protrude from the hole of the mask. In the worst case, the sample may be caught by a shutter or the like in the apparatus. is there. As described above, when directly subjecting a slag sample piece collected by a prismatic sampler to X-ray fluorescence analysis, in order to eliminate the need for sample preparation, the problem due to unevenness around the smooth analysis surface is solved. Needed.

Furthermore, the present invention is not limited to the slag specimen described above.
When a sample such as a metal sample is directly analyzed by X-ray fluorescence analysis, the analysis surface needs to be polished flat, and if an analysis method that minimizes the area to be polished is found, the time required for sample preparation can be reduced.

[0018]

SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems of the prior art, and prevents a decrease in analysis accuracy due to irregularities on the sample surface when directly performing X-ray fluorescence analysis on a solid sample piece. An object of the present invention is to provide a sample mask and a sample holder for fluorescent X-ray analysis, which are capable of performing the analysis. Furthermore, the present invention quickly analyzes slag that plays an important role in controlling the composition of steel and pig iron in the steel refining process and pig iron manufacturing process, and operates online based on the obtained analysis results. It is an object of the present invention to provide a method of X-ray fluorescence analysis of slag which can provide the guidelines of the above.

[0019]

A first invention is a sample mask 2 for X-ray fluorescence analysis having an opening 6 for irradiating primary X-rays and extracting characteristic X-rays. A sample mask for X-ray fluorescence analysis, wherein a projection 4 surrounding the opening 6 is provided on a surface opposite to the above.

A second aspect of the present invention is directed to a primary X-ray
A fluorescent X-ray analysis sample mask 1 having an X-ray extraction opening 6 and a sample X-ray analysis sample holder 1 having a sample holding jig 3 for pressing and fixing the sample on the sample mask 2; A sample holder for X-ray fluorescence analysis, wherein a projection 4 surrounding the opening 6 is provided on a surface of the mask 2 facing the sample.

In the first and second aspects of the present invention, it is preferable that the projection 4 surrounding the opening 6 is a projection that contacts the smooth surface of the sample at three or more points. This is because the protrusion 4 comes into contact with the smooth surface of the sample at three or more points, and thus the smooth surface (analytical surface) of the sample is basically obtained.
Can be set at the reference position [: reference plane (intensity calibration position)] of the fluorescent X-ray analysis.

In the first and second aspects of the present invention, the protrusion 4 surrounding the opening 6 is a protrusion having the same height at three or more points in contact with the smooth surface of the sample. Preferably, there is. This is because the sample is brought into contact with the smooth surface of the sample at three or more points having the same height, so that the smooth surface (analysis surface) of the sample is moved to the reference position [: reference surface (intensity calibration position)] for X-ray fluorescence analysis. This is because it is easier to set.

The projection 4 surrounding the opening 6 may be a continuous projection continuously contacting the smooth surface of the sample. In the above-described second invention, it is preferable that the sample contact portion of the sample holding jig 3 is formed of an elastic body (a preferred embodiment of the second invention). According to a third aspect of the present invention, there is provided a method of X-ray fluorescence analysis of slag using the sample mask for X-ray fluorescence analysis according to the first aspect of the invention, wherein the molten slag is attached to a peripheral surface of a prismatic sampler or a plate-like sampler. A slag fluorescent X-ray analysis method characterized in that the slag is separated after quenching and solidification, and a smooth analysis surface of the obtained slag sample piece is brought into contact with the projection 4 of the sample mask 2 and X-ray fluorescence analysis is performed. is there.

According to a fourth aspect of the present invention, there is provided a method for X-ray fluorescence analysis of slag using the sample holder for X-ray fluorescence analysis according to the second aspect of the present invention or the preferred embodiment of the second aspect, wherein the molten slag is formed into a prismatic shape. The sample is adhered to the peripheral surface of a sampler or a plate-like sampler, quenched, solidified, and peeled off, and the smooth analysis surface of the obtained slag sample piece is brought into contact with the projection 4 of the sample mask 2, and the slag sample piece is put into the sample. A slag X-ray fluorescence analysis method characterized by performing X-ray fluorescence analysis using the sample holder 1 after pressing and fixing with a holding jig 3.

In the third and fourth aspects of the present invention, it is preferable that the X-ray fluorescence analysis method is a bottom-side irradiation type X-ray fluorescence analysis method. Preferred Embodiment 4 of the Invention). In addition, the above-mentioned bottom surface irradiation type fluorescent X-ray analysis method refers to a method of irradiating primary X-rays from below the sample and analyzing.

In the above-described method, the sample is pressed against the sample mask disposed below the sample by gravity or both the gravity and the sample holding jig, and is fixed at the reference position.

[0027]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail. FIG. 1 shows an example of a sample mask for X-ray fluorescence analysis of the present invention by a plan view (a) and a cross-sectional view taken along the line AA (b). FIG. 2 shows an example of a sample holding jig of the sample holder for X-ray fluorescence analysis of the present invention by a plan view (a) and a sectional view taken along the line BB (b).

FIG. 3 is a sectional view showing an example of a sample mask and a sample holder for fluorescent X-ray analysis of the present invention in a state where a slag sample piece is set and fixed. 1 to 3, reference numeral 1 denotes a sample holder for X-ray fluorescence analysis (hereinafter also referred to as a sample holder), 2 denotes a sample mask for X-ray fluorescence analysis (hereinafter also referred to as a sample mask), 3 denotes a sample holding jig, and 4 denotes a sample holding jig. Protrusions, 5 an elastic body such as a spring, 6 an opening of the sample mask 2, 7 a slag sample piece, 7a an analysis surface of the slag sample piece, 7b
Is a projection of the slag sample piece, 7c is a sample surface opposite to the analysis surface of the slag sample piece, 8 is a surface of the sample mask 2 facing the sample,
9 denotes a screw.

The projection 4 is provided on a surface 8 of the sample mask 2 facing the sample, and the opening 6 of the sample mask 2 is provided.
In the case of the sample mask 2 illustrated in FIGS. 1 to 3, the protrusion 4 has a smooth surface which is a peripheral surface of the analysis surface 7a of the sample, as shown in FIG. Is a continuous protrusion that is in continuous contact with (: abuts). As illustrated in FIGS. 1 and 3, the first invention is a sample mask 2 for X-ray fluorescence analysis having an opening 6 for irradiating primary X-rays and extracting characteristic X-rays. This is a fluorescent X-ray analysis sample mask provided with a projection 4 surrounding the opening 6 on a surface facing the sample.

Further, as exemplified in FIGS.
The invention provides a fluorescent X-ray analysis sample mask 2 having an opening 6 for primary X-ray irradiation and characteristic X-ray extraction, and a fluorescent X-ray having a sample holding jig 3 for pressing and fixing a sample on the sample mask 2. A sample holder 1 for X-ray analysis, which is a sample holder for X-ray fluorescence analysis provided with a projection 4 surrounding the opening 6 on a surface of the sample mask 2 facing the sample.

According to the first and second aspects of the present invention, since positioning is performed only at the protrusion around the analysis section, even if the peripheral portion of the slag sample piece has a protrusion on the analysis surface side. ,
By providing a projection 4 having a height of several mm, for example, on the surface of the sample mask 2 facing the sample, the danger of the sample coming into contact with the holder is greatly reduced, and the projection of the slag can be removed without polishing or the like. It is possible to set the analysis surface at a reference position.

The closer the projection 4 surrounding the periphery of the opening 6 of the sample mask 2 to the focal position of the fluorescent X-ray analyzer, the more accurate the analysis can be made without attenuation of the X-ray intensity.
In a preferred aspect of the second invention, the non-analytical surface of the sample such as the slag sample 7 (the sample surface opposite to the analytical surface) is used.
Is an elastic member 5 which is an elastic member such as a spring or rubber.
The sample piece is fixed by lightly pressing through the, so that the sample holder is not shifted even when the sample holder is rotated or moved.

According to a third aspect of the present invention, there is provided a method of X-ray fluorescence analysis of slag using the sample mask for X-ray fluorescence analysis according to the first aspect of the present invention, wherein the molten slag is provided on a peripheral surface of a prismatic sampler or a plate-like sampler. This is an X-ray fluorescence X-ray analysis method for performing X-ray fluorescence analysis by bringing a smooth analysis surface of the obtained slag sample piece into contact with the protruding portion 4 of the sample mask 2 after quenching and solidifying the slag.

According to a fourth aspect of the present invention, there is provided a method of X-ray fluorescence analysis of slag using the sample holder for X-ray fluorescence analysis according to the second aspect of the invention or a preferred embodiment of the second aspect of the invention, wherein the molten slag is formed in a prismatic shape. The sample is adhered to the peripheral surface of a sampler or a plate-like sampler, quenched, solidified, and peeled off, and the smooth analysis surface of the obtained slag sample piece is brought into contact with the projection 4 of the sample mask 2, and the slag sample piece is put into the sample. This is a slag X-ray fluorescence analysis method in which X-ray fluorescence analysis is performed using the sample holder 1 after being pressed and fixed by the holding jig 3.

In the third and fourth aspects of the present invention, the above-mentioned fluorescent X-ray analysis method is a fluorescent X-ray analysis method of a bottom-side irradiation type in which primary X-rays are irradiated from below the sample and analyzed. (Preferred embodiment of the third invention, fourth embodiment)
Preferred embodiment of the invention). In the method described above, the sample is pressed by gravity against a sample mask arranged below the sample and fixed at a reference position, or using a sample holding jig brought into contact with the sample above the sample, Both the gravity and the sample holding jig press the sample mask placed below the sample to fix it at the reference position.

The above-described first to fourth inventions, preferred embodiments of the second invention, preferred embodiments of the third invention, and preferred embodiments of the fourth invention (these inventions and preferred embodiments will be referred to as the present invention hereinafter). (Collectively referred to as)), the analysis surface of the sample is desirably in a smooth state. According to the present invention, the sample is brought into contact with the sample mask for X-ray fluorescence analysis described above, inserted into an X-ray fluorescence analyzer, X-rays are irradiated on the analysis surface of the sample, and X-ray fluorescence analysis is performed. It has become possible to quickly and accurately analyze the composition of a sample such as slag.

Next, the operation and effect of the sample mask and sample holder for X-ray fluorescence analysis of the present invention will be described with reference to the drawings. FIG. 4 is a cross-sectional view showing the positional relationship between the sample mask and the slag sample when the slag sample is placed on the conventional sample mask for X-ray fluorescence analysis and the sample mask for X-ray fluorescence analysis of the present invention. .

FIG. 4 (a) shows the case where the conventional sample mask is used, and FIGS. 4 (b) and 4 (c) show the case where the sample mask of the present invention is used. This shows the positional relationship. In FIG. 4C, reference numeral 10 denotes an O-ring, and other reference numerals indicate the same contents as in FIG.

When the conventional sample mask shown in FIG. 4A is used, since the analysis surface 7a of the slag sample piece 7 is inclined, it is difficult to set a reference surface (intensity calibration position) for X-ray fluorescence analysis. . In contrast, FIG. 4 using the sample mask of the present invention.
In the case of (b), the analysis surface 7a of the slag sample piece 7 is absorbed by the distance d even if there is a convex portion at the end of the slag sample piece 7, so that it can always be accurately held on the reference surface of the sample mask 2. .

Therefore, the sensitivity can be calibrated here with the reference plane as the new reference plane position in FIGS. 4B and 4C, so that the analysis can be performed without causing an error in the actual sample. When the conventional sample mask shown in FIG. 4A is used, the sample moves when the sample is rotated, and there is a problem in analyzing the average composition of the analysis surface. By using the sample holder provided with the sample holding jig 3 for bringing the elastic body into contact with the sample contact portion, which is a preferred embodiment of the present invention, the above-mentioned problems of the prior art can be solved.

Further, in the sample mask and the sample holder of the present invention, an O-ring is interposed between the tip of the projection 4 and the smooth surface of the sample as shown in FIG. Movement can be completely prevented. Further, in the case where the fluorescent X-ray analysis of the lower surface irradiation method is performed by using an elastic O-ring made of, for example, rubber or elastic resin, the sample piece during rotation of the sample can be used without the sample holding jig 3. Movement (slip) can be prevented, and analysis can be performed.

As described above, in the present invention, the analysis surface of the sample is desirably smooth. FIG. 5 shows an example of a suitable slag sampler for preparing a slag sample in the slag X-ray fluorescence analysis method of the present invention. FIG. 5 (a) shows a longitudinal sectional view of a prismatic sampler,
FIG. 5B is a cross-sectional view taken along the line CC of FIG. 5A.

5 (a) and 5 (b), reference numeral 20 denotes iron,
A hollow prism made of metal such as stainless steel, 21 is a slag release agent, 22 is a mortar, and 23 is a paper tube. Note that the slag release agent 21 is applied to the prism in advance so that the slag after cooling and solidification can be more easily separated from the prism. In the method of X-ray fluorescence analysis of slag of the present invention, the prismatic sampler illustrated in FIG. 5 is immersed in the molten slag by a predetermined length, and the molten slag is attached to the peripheral surface of the sampler.
After the slag is cooled and solidified, it is peeled off and subjected to analysis.

In the case of analyzing slag, instead of a prismatic sampler, a sampler having at least a molten slag adhered portion may be used, and a sample for analysis may be prepared in the same manner as described above for analysis. preferable. According to the above-described method, the fluorescent X is smooth over the entire contact surface with the sampler.
Although a plate-like sample suitable as a sample for line analysis can also be obtained,
A sample in which burr-like projections are present around the slag sample piece by reflecting the shape of the corner portion of the sampler is also obtained.

In this case, the final shape of the slag specimen is often found only after the slag after cooling and solidification is peeled off. As a result, when a sample piece having burr-like protrusions formed around the slag sample piece is obtained and analysis is performed on the slag sample piece, performing operations such as polishing to remove the protrusions is a rapid analysis. It is not desirable from the aspect of sex.

The sample mask and sample holder for X-ray fluorescence analysis of the present invention have a flat surface at a predetermined position even if a projection such as a burr-like projection is present on the peripheral portion on the analysis surface side of the sample. 10 sample masks and sample holders that can be set
For example, a positioning protrusion 4 having a height of several mm is provided in a portion close to a hole for an analysis region of about 30 mmφ. As a result, at the time of analysis, the sample was not affected by the overall shape of the sample, and as a result, accurate analysis of the sample could be performed as shown in Examples described later.

In a wavelength-dispersive X-ray fluorescence spectrometer, the sample is generally rotated in order to reduce errors due to the directionality of the spectroscope. A slag piece just placed on the holder by the movement is likely to slip. For this reason, the slag sample piece is fixed by lightly pressing the sample surface, such as the slag sample piece, opposite to the analysis surface of the sample piece through an elastic body such as a spring or rubber, which is an elastic member. Even when the holder is rotated or moved, no misalignment occurs.

[0048]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below based on embodiments. Using the sample mask for X-ray fluorescence analysis, the sample holder, and the X-ray fluorescence analysis method of the present invention, the composition of slag in the refining process of steel was analyzed. That is, the molten slag in the steel refining process is sampled by the prismatic sampler shown in FIG. 5 described above, and the contact surface of the slag sample piece obtained by peeling after cooling and solidifying with the sampler is described above with reference to FIGS. Using a sample mask and a sample holder shown in FIG. 3, X-ray fluorescence analysis was performed by a bottom irradiation method.

For comparison, the conventional sample mask 2 shown in FIG. 4A has a flat surface facing the analysis surface side of the sample.
X-ray fluorescence analysis was carried out using a sample holder to which a glass bead was attached, and a glass bead was prepared for X-ray fluorescence analysis.
In the above analysis, a fundamental parameter method in X-ray fluorescence analysis was used so that the influence of the shape was minimized.

Table 1 shows the obtained analysis results.

[0051]

[Table 1]

As is clear from Table 1, the analysis results according to the present invention were in good agreement with the glass bead method, which is the standard method, as compared with the case where the conventional sample mask was used. Also, the intensity of the fluorescent X-ray itself was higher in the case of the present invention than in the case where the conventional sample mask was used. This is because, in the case of a sample holder to which a conventional sample mask is attached, the analysis surface is at a position far away from the reference surface due to a projection on the periphery of the slag sample piece, and the strength is attenuated. In the case of the sample holder, this is because the analysis surface was in good agreement with the reference surface.

In the case of a sample holder with a conventional sample mask, the analysis surface is located at a position distant from the reference surface.
It is considered that an error occurred in the analysis value. By using the method of X-ray fluorescence analysis of the sample mask, sample holder and slag for X-ray fluorescence analysis of the present invention, the analysis position of the sample can be set with high accuracy, and the analysis can be performed without moving the sample even when rotating the sample. It is possible to obtain analysis results that are in good agreement with the standard glass bead method, which is the standard method, and to perform slag composition analysis within 2 minutes, which required at least 30 minutes with the conventional glass bead method Became possible.

Further, since the sample preparation work is unnecessary, the workability as a whole is improved. As a result, rapid control of the refining process based on the reduction of the slag composition analysis time and optimization of the refining conditions based on the information on the slag composition became possible. INDUSTRIAL APPLICABILITY The present invention can be effectively used in various manufacturing processes involving slag generation, and in various manufacturing processes dealing with molten materials, other than the pig iron manufacturing process and the steel refining process.

[0055]

By using the method of X-ray fluorescence analysis of a sample mask, sample holder and slag for X-ray fluorescence analysis according to the present invention, an analysis result which is in good agreement with the conventional glass bead method as a standard method can be obtained. The slag composition analysis, which required at least 30 minutes or more in the conventional glass bead method, can be performed within 2 minutes.

Further, since the sample preparation work is not required, the whole workability is improved. As a result, rapid control of the refining process based on the reduction of the slag composition analysis time and optimization of the refining conditions based on the information on the slag composition became possible. INDUSTRIAL APPLICABILITY The present invention can be effectively used in various production processes involving slag generation, and further in various production processes dealing with a molten material, and the industrial significance thereof is great.

[Brief description of the drawings]

FIGS. 1A and 1B are a plan view and a cross-sectional view taken along line AA, respectively, showing an example of a sample mask for X-ray fluorescence analysis of the present invention.

FIG. 2 is a plan view (a) showing an example of a sample holding jig of a sample holder for X-ray fluorescence analysis of the present invention, and a cross-sectional view taken along the line BB (b).
It is.

FIG. 3 is a cross-sectional view showing an example of a sample mask and a sample holder for fluorescent X-ray analysis of the present invention in a state where a slag sample piece is set and fixed.

FIG. 4 is a sectional view (a) showing a positional relationship between a conventional sample mask and a slag sample piece, and sectional views (b) and (c) showing a positional relationship between a sample mask and a slag sample piece of the present invention. is there.

5A is a side sectional view showing an example of a slag sampler according to the present invention, and FIG.

[Description of Signs] 1 Sample holder for X-ray fluorescence analysis (: sample holder) 2 Sample mask for X-ray fluorescence analysis (: sample mask) 3 Sample holding jig 4 Projection 5 Elastic body 6 Opening of sample mask 7 Slug Sample piece 7a Analysis surface of slag sample piece 7b Projection of slag sample piece 7c Sample surface opposite to analysis surface of slag sample piece 8 Surface opposite to sample mask sample 9 Screw 10 O ring 20 Metallic hollow prism 21 Slag Release agent 22 Mortar 23 Paper tube

Continuation of the front page (72) Inventor Kimimoto Yamamoto 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba Pref. Kawasaki Steel Research Institute Co., Ltd. (72) Inventor Hideo Enyama 14-8 Akaoji-cho, Takatsuki-shi, Osaka Industry Co., Ltd.

Claims (4)

[Claims] 1. A fluorescent X-ray analysis sample mask (2) having an opening (6) for irradiating primary X-rays and extracting characteristic X-rays, the surface of the sample mask (2) facing the sample. A sample mask for X-ray fluorescence analysis, wherein a projection (4) surrounding the opening (6) is provided thereon. 2. A sample mask (2) for X-ray fluorescence analysis having an opening (6) for irradiating primary X-rays and extracting characteristic X-rays, and a sample holder for pressing and fixing the sample on the sample mask (2). A sample holder (1) for fluorescent X-ray analysis having a jig (3), a projection (4) surrounding the opening (6) on a surface of the sample mask (2) facing the sample. A sample holder for X-ray fluorescence analysis, wherein the sample holder is provided. 3. A method for X-ray fluorescence analysis of slag using the sample mask for X-ray fluorescence analysis according to claim 1, wherein the molten slag is adhered to a peripheral surface of a prismatic sampler or a plate-like sampler and solidified by rapid cooling. X-ray fluorescence X-ray analysis method for slag, wherein the slag sample is peeled off, and a smooth analysis surface of the obtained slag sample piece is brought into contact with a projection (4) of the sample mask (2) to perform X-ray fluorescence analysis. . 4. A method for X-ray fluorescence analysis of slag using the sample holder for X-ray fluorescence analysis according to claim 2, wherein the molten slag is adhered to the peripheral surface of a prismatic sampler or a plate-like sampler, and then quenched and solidified. Peeling and bringing the smooth analysis surface of the obtained slag sample piece into contact with the projection (4) of the sample mask (2), and holding the slag sample piece with the sample holding jig
(3) A method of X-ray fluorescence analysis of slag, comprising performing X-ray fluorescence analysis using the sample holder (1) after pressing and fixing in (3).