JP4738876B2 - Analytical sample preparation method and apparatus - Google Patents

Description

  The present invention removes a surface oxide layer from a specimen of iron (steel, steel and iron alloy), or a non-ferrous metal such as copper or aluminum, and its composition and impurities are obtained by X-ray fluorescence analysis or emission spectroscopic analysis. Further, the present invention relates to a method and an apparatus for preparing a sample used for analysis for confirming the content of carbon, sulfur, nitrogen and the like by gas analysis by burning steel and the like at a high temperature.

  Methods for confirming the composition and impurities of steel and non-ferrous metals in production or products by X-ray fluorescence analysis, arc emission analysis, spark emission analysis, etc. are defined by JIS, ISO, etc. (for example, JIS G1256-1982, JIS G1253, etc.). A plate-like sample having a fresh flat surface is used for these analyses.

On the other hand, gas analysis by infrared spectroscopic analysis is also performed for the purpose of confirming the content of carbon, sulfur, nitrogen, etc. in steel and non-ferrous metals in production or in products. A granular or fine sample is used for gas analysis.
The sample used for the above analysis needs to be a fresh surface and a fresh fine piece free of impurities such as oxides and contaminants.
For the preparation of these analytical samples that have been carried out conventionally, the side surface of an approximately circular rod-shaped specimen having an oxide layer on the surface is shaved with a lathe, and then rounded to a predetermined thickness with a rotating circular saw. On the other hand, a method has been used in which a sample is made into a solid sample, a hole is made in a specimen with a drill, and the generated perforated piece is made into a fine piece, or a thin piece is punched into a granular sample.

  However, in this method, since it is necessary to prepare samples with separate apparatuses, it is difficult to prepare samples for analysis having different shapes with one apparatus, and therefore automation of sample preparation. It was also difficult.

  The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an oxide layer and contaminants for X-ray fluorescence analysis and emission spectroscopic analysis of steel or non-ferrous metals and gas analysis. To provide an analytical sample preparation method and apparatus capable of simultaneously preparing a plate-shaped sample having a removed fresh surface and fresh fine pieces from which an oxide layer and contaminants have been removed with one apparatus.

According to the present invention, the analyte of rod-like or disk-like steel or non-ferrous metal section is substantially circular, and a plate-like sample having a fresh plane subjected to X-ray fluorescence analysis and / or emission spectroscopy analysis, gas analysis to the new Korea fine pieces to use in the analysis sample preparation methods for forming, the rotary head of its tapered form cutting teeth for cutting the peripheral portion of the cut surface of the specimen tapered (a) When, with the taper formed cutting teeth (a) by tapered peripheral edge cutting to a cut surface formed fine pieces formed cutting teeth to form fine pieces for gas analysis (b), it is provided Using a milling machine, the peripheral edge of the cut surface of the specimen is cut with the tapered cutting teeth (a) while rotating the rotary head on the same axis to form a tapered peripheral edge, and then the specimen Or water the milling machine While moving in the horizontal direction, by cutting the cut surface of the said specimen periphery tapered in fines formed cutting teeth (b) is formed, that you form a cutting surface and fines for analysis A featured analytical sample preparation method is provided.

Further, according to the present invention, the analyte of rod-like or disk-like steel or non-ferrous metal section is substantially circular, and a plate-like sample having a fresh plane subjected to X-ray fluorescence analysis and / or emission spectroscopy analysis, in analytical sample preparation apparatus for forming a new Korea fine pieces to use for gas analysis, and a clamp for holding the specimen, and the full rice board, is installed, the milling machine, A taper-formed cutting tooth (a) for cutting the peripheral edge of the cut surface of the specimen into a taper shape on the rotating head, and a cut surface having a tapered peripheral edge formed by the taper-forming cutting tooth (a) are cut. And a fine piece forming cutting tooth (b) for forming a fine piece for gas analysis, and the taper forming cutting tooth (a) while rotating the rotary head on the same axis. Perimeter of specimen cut surface The sample in which a tapered peripheral portion is formed by cutting a portion, and then the tapered peripheral portion is formed by the fine piece forming cutting teeth (b) while moving the sample or the milling machine in a horizontal direction. by cutting the cut surface analytical sample preparation apparatus according to claim der Rukoto capable of forming a cutting surface and a fine piece for analysis is provided.

  According to the present invention, an analysis of a steel or non-ferrous metal that can easily produce a plate-like sample having a fresh surface from which oxide layers and contaminants on the surface have been removed and a fresh fine piece with the same apparatus. A sample preparation method for analysis and an analytical sample preparation apparatus that can be automated are provided.

  The feature of the present invention is that, for example, when preparing a sample for analysis from an ingot having a substantially circular cross section of the specimen formed for analysis during the production of steel, the oxide layer is cut from the surface of the ingot to obtain a fresh surface. And a plate-like sample having a fine piece for analysis and a fresh surface can be prepared with one apparatus. The plate-like sample obtained by the present invention is used for various analyzes such as X-ray fluorescence analysis and emission spectroscopic analysis utilizing the fresh plane, and the fine piece sample is dissolved or burned. Used for gas analysis.

The present invention will be described below with reference to the drawings.
FIG. 1 shows a schematic diagram of an example of the apparatus of the present invention. In the cutting box B, in order from the left side, a specimen A having a substantially circular cross section for preparing a sample, a clamp 1 for fixing the specimen A in a vertical direction, and a rotating circle movable left and right for cutting the specimen A horizontally. A saw 2 and a milling machine 3 that moves to the left and right in conjunction with the rotary circular saw 2 and removes burrs from the peripheral portion of the cut surface formed by the rotary circular saw 2 and cuts fine pieces to smooth the cut surface. Is installed. The clamp 1 can be moved up and down with the specimen A fixed. In the milling machine 3, for example, as shown in a schematic plan view in FIG. 2, a taper-forming cutting tooth 4a is formed on the rotary cutting head 4 to deburr the peripheral edge of the cut surface of the specimen A and cut the peripheral edge into a tapered shape. And two types of cutting teeth, a fine piece forming cutting tooth 4b, which cuts the cut surface on which the tapered periphery is formed to form a fine piece for gas analysis and makes the cut surface a fresh smooth surface, is a milling machine. Removably attached to inner and outer concentric circles centering on the shaft.

  The cutting tooth 4a cuts the peripheral edge of the circular cut surface of the specimen A into a taper shape (also serves as deburring), and removes an oxide layer, contaminants, and the like from a constant width portion on the side surface below the cut surface. The cutting teeth 4b are for cutting the cut surface of the specimen A with a predetermined thickness (for example, about 20 to 50 μm) after the tapered cutting. This also makes it possible to deburr the peripheral edge.

  In the method of the present invention, for example, the specimen A is cut while moving the rotary circular saw 2 installed in the above apparatus to the left to expose a fresh cut surface, but burrs are generated at the peripheral portion of the cut surface. . In order to expose a fresh surface by cutting a part of the side surface below the deburring and specimen cutting surface, the milling machine 3 is also moved in the left direction in conjunction with the rotary circular saw 2, and the center of the specimen cutting surface and the milling machine are moved. The movement of the milling machine 3 is stopped when the rotation axis 3 coincides. Then, the peripheral portion of the specimen cutting surface is cut with the cutting teeth 4a while the rotary cutting head 4 is lowered so that the peripheral portion is cut into a tapered shape. This tapered cutting can be performed by cutting the specimen A while raising the specimen A without lowering the rotary cutting head 4, and any of them may be used in the present invention. FIG. 3 (1) shows a state where the peripheral edge of the specimen A starts to be cut into a taper shape by the cutting teeth 4a, and FIG. 3 (2) shows a state of the specimen A cut into a taper shape.

Next, in order to cut the cut surface of the specimen A on which the tapered peripheral portion is formed with the cutting teeth 4b of the rotary head 4 at a predetermined thickness, as shown in FIG. While the head 4 is lowered and the milling machine 3 is moved in the right direction, the entire cutting surface is cut in an arc shape with the cutting teeth 4b from the left peripheral portion to the right peripheral portion of the specimen. The cutting piece at this time is collected and used as a fine piece sample for analysis. FIG. 4 (2) shows the state of the specimen A after the end of cutting. The cutting with the cutting teeth 4b can be performed by raising the specimen A without lowering the rotary head, but any of them may be used in the present invention.
A smooth and fresh cut surface for analysis and a fresh fine piece sample from which the oxide layer and contaminants are removed from the specimen by cutting the cutting teeth 4a and 4b can be prepared.

  In order to perform the above cutting, the cutting teeth 4a and 4b are formed on the rotating cutting head 4 of the milling machine 3, for example, on the inner concentric circle centering on the rotation axis of the milling machine, as shown in FIG. However, at least one 4b is replaceably mounted on the outer concentric circle. For example, the cutting teeth 4a are formed in a right triangle plate shape as shown in a perspective view in FIG. 5 and the slopes thereof are processed so that the peripheral edge of the specimen A can be cut. Moreover, what installed the cutting tooth 4a on the slope of the cutting tooth 4a attachment base formed in the above-mentioned right triangle plate shape so that replacement | exchange is possible can also be used.

  After the cutting by the cutting teeth 4a is completed, the cutting surface of the specimen A whose peripheral portion is cut into a tapered shape is cut in an arc shape by the cutting teeth 4b by the rotation of the rotary cutting head 4 while the milling machine is moved to the right, for example. To do. The shape of the cutting teeth 4b is not particularly limited as long as the tip of the cutting teeth 4b is formed so as to cut a plane. Also, the cutting edge 4a of the right triangular plate-like cutting tooth 4a is processed into a shape capable of plane cutting (the one in which 4a and 4b are integrally formed), or the cutting tooth as shown in the perspective view of FIG. It is also possible to use one in which the cutting teeth 4b are replaceably installed at the lower end portion of the right triangular plate-like mounting base 4a. In the present invention, the aspect of the cutting teeth 4a and 4b is not particularly limited.

  In the above example apparatus, the rotary circular saw 2 and the milling machine 3 are used as independent cutting means and cutting means, respectively, but they can also be used as an integrated unit. For example, FIG. 7 shows an example. In the case of improving a milling machine, a circular saw 2 is first installed so as to be exchangeable, and the two types of cutting teeth 4a and 4b are provided under the circular saw 2. The thing which installed the head 4 is mentioned. The method of use is the same as in the above apparatus.

  Further, in the apparatus of the present invention, the clamp 1 holds, for example, a rod-shaped specimen A horizontally and cannot move the specimen A in the left-right direction and the up-down direction, and the rotary circular saw 2 and the milling machine 3 are interlocked. The rotary circular saw 2 rotates in the vertical direction to cut the specimen A, and the milling machine 3 is installed so that the cut surface can be cut (so-called) Horizontal milling machine), the installation direction of the clamp 1, the rotary circular saw 2 and the milling machine 3, whether up / down and left / right movements are not particularly limited. Also in this case, it is possible to use a structure in which the rotary circular saw and the milling machine are integrated. Further, in the present invention, the cutting by the rotating circular saw 2 and the milling machine 3 and the collection of the cut fine pieces can be performed in an inert gas such as nitrogen gas or argon to prevent the generation of oxide during cutting. .

  The cutting teeth 4a installed on the rotary head of the milling machine are formed on the hypotenuse of a right triangle, for example, as shown in a schematic perspective view of FIG. While cutting or lowering the rotating head, the peripheral edge of the cut surface of the specimen A is cut into a taper shape. The cutting teeth 4b are not particularly limited as long as they can cut the cut surface of the specimen A. Further, the rotary circular saw 2 has a cutting edge made of cemented carbide detachably installed at the tip, and the cutting teeth 4a and 4b are made entirely of cemented carbide or a part to be installed on the mounting base. Things can be used. For cutting and cutting steel, those made of cemented carbide are particularly preferred. These materials can be selected according to the type of specimen and are not particularly limited.

  According to the present invention, the preparation of a plate-like sample having a fresh surface from which a surface oxide layer or contaminants are removed from a specimen of steel or non-ferrous metal and a fresh fine piece can be easily prepared with the same apparatus. be able to. The apparatus of the present invention can be automatically operated by computer control.

It is a schematic diagram explaining an example of the apparatus of this invention. It is a schematic plan view explaining arrangement | positioning of the cutting teeth 4a and 4b attached to the rotary cutting head of the milling machine of this invention. (1) is a schematic diagram illustrating a process of cutting the peripheral edge of the specimen with the cutting teeth 4a. (2) is a schematic view of a specimen with a peripheral edge cut into a tapered shape. (1) Schematic diagram illustrating a process of cutting the cut surface of the specimen with the peripheral edge cut into a taper shape with the cutting teeth 4b. (2) shows a state (2) in which the cut surface of the specimen is cut smoothly. It is a schematic diagram to explain. It is a perspective view explaining the cutting tooth 4a. It is a schematic perspective view explaining the example which installed the cutting teeth 4a and 4b in the common attachment base. It is a schematic diagram explaining an example of what comprised the rotary circular saw and the milling machine integrally.

Explanation of symbols

1: Specimen holding clamp 2: Rotating circular saw 3: Milling machine 4: Rotating cutting head 4a: Taper forming cutting tooth 4b: Fine piece forming cutting tooth A: Specimen B: Cutting box

Claims (6)

Cross section from the sample of generally circular rod-like or disk-like steel or non-ferrous metals, a plate-like sample having a fresh plane subjected to X-ray fluorescence analysis and / or emission spectroscopy analysis, new to use for gas analysis Korea a fine piece, in analytical sample preparation methods for forming,
The rotary head of that, the taper forming the cutting teeth (a) cutting a peripheral portion of the cut surface of the specimen to the tapered, the cut surface tapered peripheral portion is formed by a taper formed cutting teeth (a) use a fine piece forming the cutting teeth cut to form a fine piece for gas analysis (b), the milling machine is installed,
While rotating the rotary head on the same axis, the taper forming cutting teeth (a) cut the peripheral edge of the cut surface of the specimen to form a tapered peripheral edge,
Next, while moving the specimen or the milling machine in the horizontal direction, the cut surface of the specimen on which the tapered peripheral edge is formed with the fine piece forming cutting teeth (b) is cut, analytical sample preparation wherein that you form fine pieces. The tapered form cutting teeth (a) is concentrically inwardly of said rotary head, said fine pieces forming the cutting teeth (b), before Symbol concentrically outside of the rotating head, are respectively mounted removably in a freely The analytical sample preparation method according to claim 1. The tapered form cutting teeth (a) and the fines formed cutting teeth (b), the claims are respectively detachably attached to the same cutting teeth mounting base attached to or the rotary head are formed integrally Item 2. The sample preparation method for analysis according to Item 1. Before Machinery rolling head, a rotating circular saw, with the taper formed cutting teeth in its lower (a) and the fines formed cutting teeth (b), for analysis according to claim 2 or 3 is installed Sample preparation method. Cross section from the sample of generally circular rod-like or disk-like steel or non-ferrous metals, a plate-like sample having a fresh plane subjected to X-ray fluorescence analysis and / or emission spectroscopy analysis, new to use for gas analysis Korea in analytical sample preparation apparatus for forming the fine pieces, a,
A clamp for holding the specimen, and the full rice board, is installed,
In the milling machine, a taper-shaped cutting tooth (a) for cutting a peripheral edge portion of the cut surface of the specimen into a taper shape and a tapered peripheral edge portion are formed on the rotary head by the taper-forming cutting tooth (a). Fine piece forming cutting teeth (b) for cutting the cut surface to form fine pieces for gas analysis are installed,
While rotating the rotary head on the same axis, the taper forming cutting teeth (a) cut the peripheral edge of the cut surface of the specimen to form a tapered peripheral edge,
Next, while moving the specimen or the milling machine in the horizontal direction, the cut surface of the specimen on which the tapered peripheral edge is formed with the fine piece forming cutting teeth (b) is cut, analytical sample preparation apparatus according to claim der Rukoto capable of forming a fine piece. The sample preparation device for analysis according to claim 5, wherein a rotary circular saw is attached to the rotary head, and the taper-forming cutting teeth (a) and the fine piece-forming cutting teeth (b) are attached below the rotary circular saw.

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