JP2004012336A - Metal specimen quick collection sampler and method for quickly sampling using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sampler for collecting a specimen immediately provided for a component analysis and to provide a method for sampling using the same. <P>SOLUTION: In a metal specimen quick collecting sampler having a sample case for collecting the metal specimen from a molten metal, the sample case is formed of a space splitting plate of a material which repels the molten metal for forming a pair of left and right specimen collecting spaces by partitioning the specimen collecting space between (a) a pair of left and right split sample cases having a flat specimen collecting space for quickly solidifying the molten metal invaded from an inlet passage provided at the case at one side face and (b) the pair of the left and right split sample cases. <P>COPYRIGHT: (C)2004,JPO

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention provides a metal sample used for rapid discrimination of metal components in order to perform process control quickly and accurately in a metal refining process, particularly a metal sample suitable for component analysis by a spark emission spectrometer. And a sampling method using the sampler.
[0002]
[Prior art]
In the metal refining process, a metal sample is collected by a sampler, the components are analyzed by an analytical instrument, and the components of the metal are controlled or adjusted. This management and adjustment requires quick and accurate, but in order to perform the above management and adjustment quickly and accurately, first, it is necessary to quickly collect a metal sample and quickly provide it for analysis.
[0003]
Conventionally, spark emission spectroscopy has been widely used for analysis because it can be analyzed quickly, and the analysis itself does not take much time, but from sampling to polishing to analysis. Can take a considerable amount of time. Therefore, in order to shorten the time from sampling to analysis, various samplers for quickly collecting a sample have been proposed.
[0004]
For example, Japanese Unexamined Utility Model Publication No. 6-74964 proposes a probe for collecting a molten metal sample in which a sample collecting container and a pin sample collecting container are attached to the end of a paper tube, and a disk sample and a pin sample are simultaneously sampled. Japanese Patent Application Laid-Open No. Hei 9-21795 discloses that a small block sample collection chamber is provided in addition to a sample collection chamber, and a sample to be used for emission spectroscopy or X-ray fluorescence analysis and a sample to be used for fuel gas analysis are simultaneously collected. Metal sampling devices have been proposed.
[0005]
However, since the samples collected by these samplers have a large sample diameter and a large sample thickness, it takes a considerable amount of time before cooling after collection and preparing a sample for analysis and submitting it for analysis. Thus, the sampler described above is inferior in obtaining the analysis result quickly.
[0006]
Furthermore, in the sampler, central component segregation occurs due to a difference in solidification rate at the time of cooling, a metal structure is enlarged with a delay in the solidification rate, and inclusions such as cementite are precipitated, and emission spectroscopy is performed. There is a problem in both analysis time and analysis accuracy that abnormal light emission occurs during analysis and analysis accuracy is impaired.
[0007]
However, in the metal refining process in recent years, it is essential that component management and adjustment be performed promptly and accurately. Therefore, it is strongly desired to minimize the time from sampling to obtaining analysis results. ing.
[0008]
[Problems to be solved by the invention]
An object of the present invention is to provide a sampler for collecting a sample which can be immediately subjected to component analysis and a sampling method for rapidly collecting a sample using the sampler in order to meet the above demand.
[0009]
[Means for Solving the Problems]
The present inventors have investigated the causes of the delay in analysis time and the deterioration in analysis accuracy in metal samples collected by a conventional sampler. As a result, it was found that the delay of the analysis time and the deterioration of the analysis accuracy were caused by the thick sample for analysis.
[0010]
That is, since the molten metal starts to solidify from the moment it comes into contact with the mold wall, in a conventional sampler (for example, a cylindrical sampler), the molten metal is sufficiently introduced into the interior of the sample collection container to obtain a uniform component. In order to prepare a sample, the thickness of the sample had to be increased, but it was found that this was a cause of a delay in analysis time and a deterioration in analysis accuracy.
[0011]
Therefore, the present inventor studied the structure of a sampler capable of reducing the sample thickness to the minimum and rapidly collecting a metal sample capable of maintaining at least the analysis accuracy of the related art. In order to reduce the sample thickness, it is conceivable to first reduce the thickness of the sample collection container.However, when the sample collection container is thinned, it becomes difficult to quickly and smoothly introduce the molten metal into the sample collection container. is assumed.
[0012]
Based on this, the present inventor also examined the material of members constituting the sampler in the study of the structure of the sampler.
[0013]
As a result, the present inventor has constructed a part of the sample case body (sample collection container) from a member made of a material that is resistant to thermal shock, has excellent heat resistance, has a small amount of metal impurities, and repels molten metal. Utilizing the property of "repelling molten metal" of the member, the molten metal was quickly and smoothly penetrated to every corner of the sampling container, and the penetrated molten metal was brought into contact with the mold wall of the sampling container. We succeeded in obtaining a thin metal sample by solidifying it instantaneously.
[0014]
In addition, the inventor tried various members for members made of a material that is resistant to thermal shock and excellent in heat resistance, has a small amount of metal impurities, and repels molten metal, but when the molten metal is molten steel, quartz is used. Glass is preferred. In addition to quartz glass, for example, glass, boron nitride, and a high-temperature wet / release material (for example, ceramic powder such as boron nitride, silica, alumina, zirconia, and silicon carbide) are applied to the surface layer of a metal plate or a ceramic plate. It was also confirmed that the obtained material could be used as the above member.
[0015]
In addition, in the past, in many cases, only one sample was prepared in the sample collection container. However, this has the inconvenience that if the sample collected is defective, the sample must be collected again. At the same time, the inventor has studied the means for solving the above-mentioned inconvenience and the factor for preventing the analysis from being speeded up.
[0016]
As a result, if two sample forming chambers are provided in the sample collection container and two samples (one is a copy sample) are prepared at the same time, it is not necessary to re-collect even if one of the samples is defective. The idea was that the inconvenience of the analysis could be eliminated and the factors that hinder the speed of analysis could be eliminated.
[0017]
The present invention is based on the above idea and the result of the study, and the gist is as follows.
[0018]
(1) In a sampler provided with a sample case body for collecting a metal sample from molten metal, the sample case body is
(A) a pair of left and right half sample cases provided on one side surface with a flat sample collection space for rapidly cooling and solidifying molten metal entering from an inflow channel provided in the case body;
and,
(B) A space division of a material repelling molten metal, which is located between the pair of left and right half sample cases and divides the sample collection space to form a pair of left and right sample collection spaces in the sample case body. Board,
A metal sample rapid sampling sampler comprising:
[0019]
(2) The sampler according to (1), wherein the half sample case is made of a material having a high heat removal ability.
[0020]
(3) The material according to (2), wherein the material having a high heat removal ability is a material composed of one or more of iron, steel, aluminum, copper, and stainless steel. Metal sample rapid sampling sampler.
[0021]
(4) The metal sample rapid as described in any of (1) to (3) above, wherein the space dividing plate is a plate made of a material having excellent thermal shock resistance and heat resistance and having a small amount of metal impurities. Collection sampler.
[0022]
(5) The sampler according to (4), wherein the plate having a small amount of metal impurities is a quartz glass plate.
[0023]
(6) The sampler according to any one of (1) to (5), wherein the thickness of the sampling space is 0.5 to 20 mm.
[0024]
(7) The sampler according to any one of (1) to (6), wherein the sampling space has a substantially circular planar shape.
[0025]
(8) The sampler according to any one of (1) to (7), wherein the sampling space has a gas vent hole.
[0026]
(9) The sampler according to any one of (1) to (8), wherein the sample case body is attached to a tip of a paper tube.
[0027]
(10) In a sampling method for immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any of (1) to (9) above in a molten metal;
(B) Rapidly solidifying molten metal intruding from the inflow channel in a pair of sampling spaces divided into right and left by the space dividing plate;
(C) Pull up the sampler, quench the sample case body, and take out the metal sample.
A rapid sampling method characterized by the above-mentioned.
[0028]
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention will be described in detail. FIG. 1 shows the basic structure of a sampling container according to the present invention. The sample case body 1 has an inflow channel 5 into which the molten metal flows (this inflow channel 5 is connected to an inflow hole 8 as shown in FIG. 2). A pair of left and right half sample cases 2 each having a flat sample collecting space 4 on one side for rapidly cooling and solidifying the intruding molten metal are united with a space dividing plate 3 made of a material repelling molten metal therebetween. ing.
[0029]
Therefore, in the sample case body 1, a flat sample collection space 4 is formed on the left and right by the left and right half sample cases 2 and the space partition plate 3.
[0030]
The half sample case 2 is made of a material having a high heat removal capability in order to rapidly and rapidly solidify the molten metal and obtain a metal sample having a uniform solidified structure. As a material having a high heat removal ability, a material composed of one or more of iron, steel, aluminum, copper, and stainless steel can be used.
[0031]
The material of the half sample case may be appropriately selected in consideration of the type, characteristics, and temperature of the molten metal, and contamination and erosion by the molten metal. According to the experimental results of the present inventors, when the molten metal is molten steel, iron or steel is preferable.
[0032]
As shown in FIG. 1, it is preferable to provide a gas vent hole 6 in the sampling space 4 in order to quickly and smoothly introduce the molten metal into the sampling space 4.
[0033]
In the present invention, a plate made of a material that repels molten metal is used as the space dividing plate 3. The space dividing plate 3 is desirably a plate made of a material that is resistant to thermal shock, has excellent heat resistance, and has a small amount of metal impurities, in addition to a material that repels molten metal.
[0034]
According to the experimental results of the present inventor, as a space dividing plate, a quartz glass plate, a glass plate, a boron nitride plate, and a high-temperature wet / release material (for example, boron nitride, silica, etc.) , Alumina, zirconia, silicon carbide, or other ceramic powder).
[0035]
The space dividing plate may be made of an appropriate material in consideration of the type, characteristics, and temperature of the molten metal, and contamination and erosion of the molten metal. For example, when the molten metal is molten steel, a quartz glass plate is suitable.
[0036]
In the present invention, the flat sample collection space 4 and the space dividing plate 3 work together in an important manner, and a metal sample that can be immediately used for analysis can be prepared. This operation will be described.
[0037]
FIG. 2 shows a cross section of one embodiment of the sample case body 1 when the sampler is immersed in the molten metal. The pair of left and right half sample cases 2, 2 sandwiching the space dividing plate 3 therebetween are firmly united by a half fixing ring 7. An inflow hole 8 connected to the inflow passage 5 for the molten metal is provided at a lower portion of the sample case body 1, and the inflow hole 8 is covered with a protective cap 9 for avoiding slag.
[0038]
When the sample case body 1 is immersed in the molten metal, the slag avoiding protection cap 9 melts and disappears due to the heat of the molten metal, and the molten metal enters through the inflow hole 8, passes through the half fixing ring 7, and inflows. From the path 5, it enters the sampling space 4.
[0039]
In this intrusion, since the space dividing plate 3 made of a material that repels molten metal is sandwiched between the half sample cases 2, the sample case body 1 is melted by the action of this “repels molten metal” property. The metal is quickly and smoothly penetrated into every corner of the sampling space 4 without solidifying near the insertion port of the sampling space 4, and after the penetration, since the sampling space 4 is flat, Immediately, the molten metal can be rapidly solidified.
[0040]
At this time, if the gas vent hole 6 is provided in the sample case body 1, when the molten metal enters, the gas inside the sampling space is discharged from the gas vent hole 6, and the molten metal enters more quickly. It is performed smoothly.
[0041]
In this way, a thin metal sample having a uniform solidified structure can be quickly obtained.
[0042]
Since the thickness of the sampling space 4 is directly reflected on the thickness (thinness) of the sample, it is important in obtaining a sample that can be immediately analyzed. When the thickness of the sampling space 4 is increased, the time until the molten metal is completely solidified is delayed, and component segregation is likely to occur.
[0043]
When the sample is subjected to gas analysis or the like, the sample may be subjected to processing such as punching or punch press. However, if the sample is too thick, unnecessary sample preparation such as cutting the sample again is required. A step is required, and in such a case, the time required from sampling to analysis cannot be reduced.
[0044]
On the other hand, when the thickness of the sampling space is reduced, it is difficult to quickly and smoothly enter the molten metal, which hinders quick collection of the metal sample.
[0045]
Therefore, there is an optimum range for the thickness of the sampling space, but this optimum range naturally depends on the type, composition, melting temperature, and the like of the metal. For example, when the molten metal is molten steel, the above-mentioned optimal range is 0.5 to 20 mm, preferably 2 to 5 mm.
[0046]
The planar shape of the sampling space 4 is not limited to a specific shape, but is substantially circular or elliptical in that the rapid solidification rate is maintained substantially constant over the entire surface of the sample and a uniform solidified structure is secured. It is preferable that
[0047]
Here, FIG. 3 shows one embodiment of the entire sampler for rapidly collecting metal samples according to the present invention. In this sample case body 1, a half fixing ring 7 that combines the half sample cases 2 and 2 is covered with a refractory material 10, and is protected from contamination and erosion by molten metal.
[0048]
The sample case body 1 is connected to a paper tube 14 with a ceramic wool 11 interposed therebetween, and is supported by a holding support rod 13. The lower portion of the holding support rod 13 is covered with the refractory ceramics 12 to protect it from contamination and erosion by the molten metal.
[0049]
In the present invention, the metal sample rapid sampling sampler shown in FIG. 3 is immersed in a molten metal, and a metal sample to be analyzed is collected.
[0050]
The metal sample rapid sampling sampler is immersed in the molten metal, and the molten metal that has entered from the inflow passage is rapidly solidified in the pair of sample collecting spaces 4 divided into right and left by the space dividing plate. The case body 1 is rapidly cooled, and an impact is applied to the tip of the case body 1 so that the space partition plate and the half sample case are separated, and a target metal sample is taken out.
[0051]
After taking out the metal sample, it is subjected to polishing and then, for example, to an emission spectrometer to analyze components.
[0052]
According to the rapid sampling method of the present invention, when the metal sample rapid sampling sampler is pulled up, the molten metal has already solidified and the metal sample has been formed inside the sampling space 4, so that after the sampler is pulled up, It is only necessary to cool the sample case body 1 to room temperature and take out the metal sample, and it is possible to greatly reduce the time required from the sampling of the metal sample to the polishing and analysis.
[0053]
Further, according to the rapid sampling method of the present invention, two identical metal samples can be sampled at the same time, so that either one can be selected as an optimal analysis target sample, and one metal sample is a solidified tissue. Even if it is defective in point, one of the metal samples can be used, so that there is no need for the trouble of collecting the metal sample again, and there is no impediment to the speed from the sampling to the polishing and analysis.
[0054]
【Example】
Next, examples of the present invention will be described, but the present invention is not limited to the conditions employed in the examples.
[0055]
(Example)
Using a half sample case having a circular sampling space having a diameter of 30 mm and a thickness of 4 mm, a metal sample rapid sampling sampler having the structure shown in FIG. 3 was prepared, and the rapid sampling method of the present invention (the method of the present invention) was used. The molten steel was sampled by the conventional sampling method (conventional method), and the analysis time and the analysis accuracy in both methods were compared.
[0056]
Regarding the analysis time, it was confirmed that the conventional method required about 120 seconds to take out the sample, while the method of the present invention could take out the sample after about 60 seconds.
[0057]
Regarding the analysis accuracy, the amount of Ti was analyzed by emission spectroscopy and compared. The result is shown in FIG. As shown in the figure, since the Ti content in both samples obtained by the method of the present invention and the conventional method has a corresponding relationship, the sample obtained by the method of the present invention is the same as the sample obtained by the conventional method in terms of analytical accuracy. Therefore, it can be seen that the method of the present invention can replace the conventional method.
[0058]
As described above, according to the sampling method of the present invention, an appropriate sample that can be immediately provided for emission spectroscopy can be quickly collected.
[0059]
【The invention's effect】
According to the present invention, when the metal sample rapid sampling sampler is pulled up, the molten metal is rapidly solidified inside the sample collection space to form a metal sample, so the sampler is pulled up from the molten metal and then cooled to room temperature. It is only necessary to take out the metal sample and then the time required from sample collection to polishing and analysis can be greatly reduced, and it is possible to quickly respond to component management and adjustment in the refining process.
[0060]
Further, according to the present invention, since the structure of the collected metal sample is refined by rapid solidification, there is no abnormal light emission during emission spectroscopic analysis, and the components of the metal sample can be analyzed with high accuracy. It is possible to respond appropriately to component management and adjustment in the process.
[0061]
Furthermore, according to the present invention, two of the same metal samples can be collected at the same time, so that either one can be selected as an optimum analysis target sample, and one metal sample can be selected in terms of a solidified structure. Even if it is defective, one of the metal samples can be used, so that the quickness required for component management and adjustment in the refining process can be maintained.
[0062]
Therefore, the present invention has a remarkable effect in quick and appropriate control and adjustment of components in the refining process.
[Brief description of the drawings]
FIG. 1 is a view showing a basic structure of a sample case body according to the present invention. FIG. 1A is a diagram showing a cross section of the sample case body, and FIG. 1B is a diagram showing a cross section taken along AA in FIG. 1A.
FIG. 2 is a diagram showing a cross section of one embodiment of a sample case body when actually immersing in a molten metal.
FIG. 3 is a view showing one embodiment of the entire sampler for rapidly collecting metal samples according to the present invention.
FIG. 4 is a diagram showing the correspondence between the amounts of Ti in both samples collected by the method of the present invention and the conventional method.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Sample case body 2 ... Half sample case 3 ... Space partition plate 4 ... Sampling space 5 ... Inflow path 6 ... Gas vent hole 7 ... Half fixing ring 8 ... Inflow hole 9 ... Protective cap 10 ... Refractory material 11 ... Ceramic wool 12 ... refractory ceramic 13 ... support rod 14 for holding ... paper tube

Claims (10)

In a sampler including a sample case body for collecting a metal sample from molten metal, the sample case body is
(A) a pair of left and right half sample cases provided on one side surface with a flat sample collection space for rapidly cooling and solidifying molten metal entering from an inflow channel provided in the case body;
and,
(B) A space division of a material repelling molten metal, which is located between the pair of left and right half sample cases and divides the sample collection space to form a pair of left and right sample collection spaces in the sample case body. Board,
A metal sample rapid sampling sampler comprising: The sampler according to claim 1, wherein the half sample case is made of a material having a high heat removal capability. 3. The metal sample according to claim 2, wherein the material having a high heat removal ability is a material composed of one or more of iron, steel, aluminum, copper, and stainless steel. 4. sampler. The sampler according to any one of claims 1 to 3, wherein the space dividing plate is a plate made of a material having excellent thermal shock resistance and heat resistance and having a small amount of metal impurities. The sampler according to claim 4, wherein the plate having a small amount of metal impurities is a quartz glass plate. The sampler according to claim 1, wherein the thickness of the sampling space is 0.5 to 20 mm. 7. The sampler according to claim 1, wherein the sampling space has a substantially circular planar shape. The sampler according to any one of claims 1 to 7, wherein the sampling space has a vent hole. The sampler according to any one of claims 1 to 8, wherein the sample case body is attached to a tip of a paper tube. In a sampling method of immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any one of claims 1 to 9 in a molten metal;
(B) Rapidly solidifying molten metal intruding from the inflow channel in a pair of sampling spaces divided into right and left by the space dividing plate;
(C) Pull up the sampler, quench the sample case body, and take out the metal sample.
A rapid sampling method characterized by the above-mentioned.

Images