JP7018804B2 - Method for preparing a sample-embedded resin for analysis - Google Patents

Description

The present invention relates to a method for preparing a sample-embedded resin for analysis by embedding and fixing a minute granular sample to be analyzed in a resin material prior to analysis, and in particular, in a resin material. It proposes a technique for improving the dispersibility of a granular sample.

For example, the element content, particle size distribution, unit separation degree, etc. of a granular sample consisting of ore, slag, sludge, dust, recycled raw materials such as electrical and electronic equipment, and other particles with non-uniform composition and particle size are measured and analyzed. Since the particles constituting the granular sample are very small, it is generally practiced to embed the granular sample in a resin material and fix it to obtain a sample-embedded resin before setting it in an analyzer. ing. As an example of such an analyzer, a mineral analysis system (Minal Liberation Analyzer, MLA) analyzes ore particles based on SEM-EDS, and is particularly used in the field of mineral resources.

In such a sample-embedded resin, in order to improve the analysis accuracy, agglomeration of particles of the granular sample in the resin material is removed as much as possible, the granular sample is sufficiently dispersed in the resin material, and the composition has a representative composition without separation and segregation. Is required.
Therefore, conventionally, when preparing a sample-embedded resin, first, the granular sample is sieved and separated into upper and lower sieves, and then they are further mixed, and the mixed sample is combined with the liquid resin material. Put it in a container, stir the inside of the container manually, defoam the liquid resin material using a vacuum desiccator, stir the inside of the container with an ultrasonic stirrer, and then cure the liquid resin material in the atmosphere. I was supposed to let you. Further, here, in order to improve the dispersibility of the granular sample in the sample-embedded resin, graphite may be charged into the container prior to charging the liquid resin material, and this may be mixed with the granular sample. Further, a cross section may be prepared and measured.

However, even if the sample-embedded resin was prepared in this way, when analyzed by the analyzer, there was not a small amount of agglomeration of fine particles, and the agglomeration could not be sufficiently suppressed, so that the analyzer agglomerated. There is a problem that it is undeniable that the analysis accuracy is lowered due to the misidentification of the particles as one particle. In addition, the above-mentioned preparation method requires a lot of time and labor to prepare the sample-embedded resin, and also involves manual work. Therefore, the granular sample of the sample-embedded resin to be produced is dispersed according to the operator. There will be variations in sex. Moreover, despite such efforts, agglomeration of small particles could not be sufficiently prevented.

Here, in the item of the conventional technique of Patent Document 1, when measuring or evaluating the properties of magnetic materials, metal powder injection molding materials and various other powders, in particular, powders such as magnet raw material powders are used in particle units. It is described that the powder to be observed is dissolved in a solvent such as water, alcohol, liquid resin, oil, etc. for separation, and ultrasonic vibration is applied in some cases.

Japanese Unexamined Patent Publication No. 7-43275

However, as described above, the agglomeration of particles cannot be reliably eliminated by applying ultrasonic vibration as described in Patent Document 1, so that the dispersibility is insufficient for analysis with higher accuracy. It becomes. In addition, washing with ethanol, solid-liquid separation, and drying are time-consuming and increase the work man-hours before analysis.

An object of the present invention is to deal with such a problem of the prior art, and an object thereof is to sufficiently suppress the aggregation of particles of the granular sample in the resin material and to sufficiently suppress the aggregation of the particles of the granular sample in the resin material. It is an object of the present invention to provide a method for producing a sample-embedded resin for analysis, which can improve the dispersibility of the sample.

As a result of diligent studies, the inventor effectively suppressed the aggregation of particles by using a rotation / revolution stirrer for mixing and stirring the granular sample and the liquid resin material put into the container, and the agglomeration of the particles was effectively suppressed in the resin material. It has been found that the dispersibility of the granular sample can be effectively improved and a representative composition without separation and segregation can be obtained. This is because the particles containing the granular sample and the liquid resin material are revolved while rotating, and the agglomeration of particles during curing of the liquid resin material is suppressed based on the mutual effect of swirl flow and vertical convection. In addition, the particles of the granular sample are kneaded with a rotating and revolving stirrer to strip off other particles adhering to the particle surface, and the temperature rises due to frictional heat. However, the present invention is not limited to such a theory.

Based on this finding, in the method for producing a sample-embedded resin for analysis of the present invention, a granular sample to be analyzed, which is composed of particles having a non-uniform particle size and contains a plurality of types of simple substances and / or compounds, is embedded in a resin material. A method for producing a sample-embedded resin in which the granular sample is fixed in the resin material. The granular sample is put into a container together with the liquid resin material, and the granular sample and the liquid resin material are contained. The container is rotated in the direction opposite to the rotation while rotating with a rotation / revolution stirrer to stir the granular sample and the liquid resin material in the container, and then the liquid resin material is cured. The initial stage of stirring by the rotation / revolution stirrer is an atmospheric atmosphere, and at least the final stage thereafter is a vacuum atmosphere .

Further, in the method for producing a sample-embedded resin for analysis of the present invention, a granular sample to be analyzed, which is composed of particles having a non-uniform particle size and contains a plurality of types of simple substances and / or compounds, is embedded in a resin material and the resin is prepared. A method for producing a sample-embedded resin in which the granular sample is fixed in a material. The granular sample is put into a container together with the liquid resin material, and the granular sample and the container containing the liquid resin material are placed in a container. The granular sample and the liquid resin material in the container are agitated by rotating in the same rotation direction as the rotation while rotating with the rotation / revolution stirrer, and then the liquid resin material is cured, and the rotation / revolution stirrer is used. The initial stage of stirring is the air atmosphere, and at least the final stage thereafter is the vacuum atmosphere .

Here, the revolution speed at the time of stirring by the rotation / revolution stirrer is preferably 400 rpm to 2000 rpm.

It is effective that the stirring time by the rotation / revolution stirrer is 1 minute to 30 minutes.

In the method for producing a sample-embedded resin for analysis of the present invention, it is preferable that the time from stirring with a rotating revolution stirrer to the completion of curing of the liquid resin material is 30 minutes to 60 minutes.

By the way, the ratio of the granular sample to the liquid resin material to be put into the container is preferably 100% by volume to 300% by volume.

In the method for producing a sample-embedded resin for analysis of the present invention, the particles constituting the granular sample can be used as ore particles.

In the method for producing a sample-embedded resin for analysis of the present invention, a container in which a plurality of containers containing a granular sample and a liquid resin material are arranged can be used as the container to be rotated by a rotation / revolution stirrer.

According to the method for producing a sample-embedded resin for analysis of the present invention, the container containing a granular sample and a liquid resin material is revolved while rotating with a rotating / revolving stirrer to stir the inside of the container into a liquid state. Since the granular sample is dispersed in the resin material and then the liquid resin material is cured, the aggregation of the particles of the granular sample in the resin material is sufficiently suppressed, thereby improving the dispersibility of the granular sample in the resin material. Can be improved.

It is a perspective view which shows the state at the time of revolving while rotating the container containing a granular sample and a liquid resin material in one Embodiment of this invention. It is a perspective view which shows the state when the container containing a granular sample and a liquid resin material is revolved while rotating in another embodiment. It is a perspective view schematically showing the state of revolving while rotating a container in which a plurality of containers containing a granular sample and a liquid resin material are arranged in still another embodiment. It is a graph which shows the particle size distribution of the granular sample which was embedded and fixed in the sample embedding resin prepared by using the crude preparation of Example, together with the particle size distribution by the particle size distribution meter of the granular sample before embedding. It is a graph which shows the particle size distribution of the granular sample which was embedded and fixed in the sample embedding resin prepared by using the crude concentrate of an Example, together with the particle size distribution by the particle size distribution meter of the granular sample before embedding. It is a graph which shows the particle size distribution of the granular sample which was embedded and fixed in the sample embedding resin prepared using the primary selection concentrate of Example, together with the particle size distribution by the particle size distribution meter of the granular sample before embedding. It is a backscattered electron image and a mineral species map of the surface of the sample embedding resin prepared by the manual stirring method using the rough selection ore of an Example. It is a back electron image and a mineral species map of the cross section and the surface of the sample embedding resin prepared by the mixer stirring method using the rough selection ore of the example. It is a backscattered electron image and a mineral species map of the surface of the sample embedding resin prepared by the manual stirring method using the crude concentrate of an Example. It is a backscattered electron image and a mineral species map of the surface of the sample embedding resin prepared by the mixer stirring method using the crude concentrate of an Example. It is a backscattered electron image and a mineral species map of the surface of the sample embedding resin prepared by the manual stirring method using the primary selection concentrate of an Example. It is the back electron image and the mineral species map of the cross section and the surface of the sample embedding resin prepared by the mixer stirring method using the primary selection concentrate of an Example.

Hereinafter, embodiments of the present invention will be described in detail.
In the method for producing a sample-embedded resin for analysis according to an embodiment of the present invention, a granular sample to be analyzed, which is composed of particles having a non-uniform particle size and contains a plurality of types of simple substances and / or compounds, is embedded in the resin material. Then, in producing a sample-embedded resin in which the granular sample is fixed in the resin material, the granular sample is put into a container together with the liquid resin material, and then the granular sample and the liquid resin material are contained. The granular sample and the liquid resin material in the container are stirred by rotating the container in a rotation direction opposite to the rotation or in the same rotation direction as the rotation while rotating the container with a rotation / rotation stirrer. , Curing the liquid resin material.

(Granular sample)
The granular sample to be analyzed shall be made into relatively small particles by subjecting ore, slag, sludge, dust, or its recycled raw materials including electrical and electronic equipment to a predetermined treatment. Can be done. Since such a granular sample is usually not intentionally homogenized in composition and particle size, it is composed of many kinds of non-uniform particles having different compositions and different particle sizes.

In particular, when targeting granular samples consisting of ore particles, such ore particles may contain copper ore, which may include, for example, chalcocite, covellite, chalcopyrite, copper ore, enargite, etc. Brochan copper ore and the like may be included. In addition to copper ore, pyrite, magnetite, silicate minerals, molybdenite, gold particles and the like can also be contained. The silicate minerals include orthoclase, albite, plagioclase, muscovite, biotite, quartz and the like.

When targeting a granular sample consisting of slag, the slag itself has a complex composition containing SiO ₂ , CaO, Al ₂ O ₃ , FeO, Fe ₃ O ₄ , etc., and the slag further contains matte particles and metal particles. In some cases.
In the case of a granular sample made of an electric / electronic device, there are particles having various compositions such as a resin part contained in the substrate, a metal part constituting a circuit, and a flame retardant part.
Sludge and dust are unlikely to have a single composition.

The particle size of the particles constituting the granular sample is, for example, in the range of 1 μm to 700 μm, typically 20 μm to 200 μm, and is relatively generally distributed and non-uniform. The particle size that can be measured by the particle size distribution meter may be, for example, 0.243 μm to 2000 μm, but the particle size of the granular sample as described above is unevenly distributed in this range.

(Resin material)
As the resin material for embedding and fixing the above-mentioned granular sample, various materials can be used as long as they can be maintained in a liquid state at the time of charging into a container and at the time of stirring, which will be described later, and can be cured thereafter. However, for example, epoxy resin, acrylic resin, phenol resin and the like can be mentioned, and among these, epoxy resin which is a thermosetting resin is preferable. Since acrylic resin is vulnerable to electron beam irradiation, the amount of current cannot be increased, which takes time for measurement, and phenolic resin may contain something other than resin, which is the measurement sample. This is because there is a concern that it cannot be determined.

(Method for preparing a resin for implanting a sample for analysis)
In order to prepare a sample-embedded resin for analysis from the above-mentioned granular sample and resin material, first, the granular sample 2 is liquid in a predetermined container 1 such as a bottomed cylindrical shape as exemplified in FIGS. 1 and 2. It is charged together with the resin material 3.
Further, here, if necessary, a resin curing agent for curing the liquid resin material 3 such as an epoxy resin by heating after stirring can be used. In this case, the liquid resin material 3 and the resin curing agent can be mixed and mixed in advance in a predetermined ratio, and the liquid resin material 3 and the resin curing agent can be put into the container 1 together with the granular sample 2. As the resin curing agent, known ones suitable for the type of the liquid resin material 3 can be used.

In this embodiment, as will be described later, the granular sample 2 can be sufficiently dispersed in the liquid resin material 3 by a rotation / revolution stirrer, so that it is not necessary to further add graphite or the like. That is, only the granular sample 2 and the liquid resin material 3 can be put into the container 1 except for the resin curing agent. Further, here, it is possible not to manually stir the granular sample 2 and the liquid resin material 3 in the container 1 by ultrasonic waves. Further, it is not necessary to perform the conventional sieving of the granular sample 2 before putting it into the container 1. Therefore, in this embodiment, the work required for producing the sample-embedded resin can be dramatically simplified, the work man-hours can be reduced, and the work time can be shortened.

The ratio of the granular sample 2 to the liquid resin material 3 to be put into the container 1 is preferably 100% by volume to 300% by volume. More preferably, it is 200% by volume to 300% by volume. That is, if the ratio of the granular sample 2 is too small, the particles may agglomerate, and if the ratio of the granular sample 2 is too large, the particles cannot be solidified, and the surface to be measured is exposed during polishing. This is because there is a concern that it will be damaged.

Next, the container 4 containing the granular sample and the liquid resin material is set in a predetermined rotation / revolution stirrer, and based on the function of the rotation / revolution stirrer, the granular sample is shown by an arrow in each of FIGS. 1 and 2. And the container 4 containing the liquid resin material is rotated and revolved at the same time to stir the granular sample 2 and the liquid resin material 3 in the container 1. More specifically, the bottom of the bottomed cylindrical container 1 is arranged so as to incline its central axis toward the diagonally downward side, and the container 4 containing the granular sample and the liquid resin material is arranged with the central axis as the rotation axis. Along with the rotation, the revolution axis is set so that the rotation axis tilts at a predetermined angle θ at a distance from the container 1, and the container 4 containing the granular sample and the liquid resin material is rotated around the revolution axis.

As a result, the bubbles in the liquid resin material 3 are pushed out by the swirling flow and the vertical convection generated by the interaction between the rotation and the revolution, and the granular sample 2 and the liquid resin material 3 are stirred without entraining the bubbles. , The dispersion can be promoted. Moreover, here, the temperature rises due to the frictional heat with the liquid resin material 3 and particles during stirring by the planetary rotation mixer, and the liquid resin material 3 is slightly cured. Therefore, the liquid resin material as described later. In addition to shortening the time required to cure No. 3, such slight curing can suppress the bias of the presence of particles due to the difference in the degree of sedimentation of the particles of the granular sample 2 inside.

The rotation / revolution agitator is not particularly limited as long as it can perform such rotation and revolution of the container 4 containing the granular sample and the liquid resin material, and for example, a known one can be used. The rotation and rotation of the rotation / revolution stirrer can be opposite to each other as shown in FIG. 1, or can be in the same rotation direction as shown in FIG. That is, the relative rotation direction of the revolution and the rotation is not particularly limited, and can be appropriately set according to the rotation / revolution agitator to be used, the state of the granular sample 2 or the liquid resin material 3, and the like.

Further, as shown in FIG. 3, a container 4a in which a plurality of containers 4 containing a granular sample and a liquid resin material are arranged can be rotated and revolved. This container 4a, which may also be called a table depending on the rotation / revolution stirrer, can also be regarded as a container containing a granular sample and a liquid resin material. In this case, the container 4a is rotated around the central axis of the container 4a as a rotation axis, the revolution axis is set so that the rotation axis is tilted at a predetermined angle θ, and the container 4a is rotated around the revolution axis. In FIG. 3, four containers 4 containing a granular sample and a liquid resin material are arranged around the central axis of the container 4a at equal intervals, but the granular sample and the liquid state in the container 4a are arranged. The arrangement mode and number of the containers 4 containing the resin material are not limited to this. By rotating and revolving the container 4a in which a plurality of containers 4 containing the granular sample and the liquid resin material are arranged in this way, the plurality of granular samples and the granular sample 2 of the container 4 containing the liquid resin material can be obtained at one time. Since it can be dispersed, work efficiency can be greatly improved.

Here, the revolution speed at the time of stirring by the rotation / revolution stirrer is preferably 400 rpm to 2000 rpm. If the revolution speed is too slow, there is a concern that aggregated grains will be formed, while if the revolution speed is too fast, the grains may wear due to friction. From this point of view, the revolution speed is preferably 400 rpm to 2000 rpm.

Further, here, the ratio of the rotation speed to the revolution speed at the time of stirring by the rotation revolution stirrer may be within a range in which vertical convection of the resin is generated and the particles do not wear each other, for example, 0.4 to 0.4 to the revolution speed. It is preferable to set it to 0.6 times. If the rotation speed is too slow, it is possible that aggregates are present because vertical convection does not occur. On the other hand, if the rotation speed is too fast, the speeds of the spiral flow and the vertical convection become high, and there is a concern that the particles will wear and differ from the original particle size.
The above-mentioned revolution speed and rotation speed can be set by the rotation revolution agitator.

The angle θ of the rotation axis during stirring by the rotation / revolution stirrer is preferably 30 ° to 60 °, more preferably 40 ° to 50 °, and the rotation axis is tilted from the revolution axis for stirring. Can be done. If the tilt angle θ of the rotation axis is small, the one with a large specific gravity tends to settle at the bottom of the container, and if the tilt angle θ is large, resin may spill from the container and the required amount of resin may not be filled in the container. There is sex. The inclination angle θ can be appropriately set according to the properties of the material.

By the way, in the stirring by the rotation / revolution stirrer as described above, the atmosphere around the container 4 containing the granular sample and the liquid resin material can be set as a vacuum atmosphere to remove microbubbles that may be mixed in the liquid resin material 3. It is suitable in that it can be done. Such microbubbles are one of the factors that cause agglomeration of particles. By stirring in a vacuum atmosphere with a rotating revolution stirrer, the use of a vacuum desiccator that has been used so far to remove microbubbles is used. Can be omitted. In the case of a vacuum atmosphere, the maximum ultimate vacuum degree can be, for example, 1.0 kPa or less, preferably 0.67 kPa or less, from the viewpoint of effectively removing microbubbles. Even if the pressure is further reduced, the effect does not change so much, and it takes time to reach such a low pressure.

However, if the surroundings of the granular sample and the container 4 containing the liquid resin material in the rotating / revolving and revolving stirrer are set to a vacuum atmosphere from the initial stage of stirring in which the granular sample 2 is hardly dispersed in the liquid resin material 3, the container can be used. There is a concern that the granular sample 2 existing near the surface of the opening of 1 may be scattered. In order to prevent this, it is preferable to perform stirring under the action of gravity as an atmospheric atmosphere in the initial stage of stirring, and then switch to a vacuum atmosphere for further stirring. That is, it is preferable that the initial stage of stirring is an atmospheric atmosphere, and at least the final stage thereafter is a vacuum atmosphere.
Here, the initial stage of stirring can be from the start time of stirring by the rotation / revolution stirrer to the time when 30 seconds to 60 seconds have elapsed. After that, the time for creating a vacuum atmosphere can be 60 seconds to 30 minutes.

The stirring time by the rotation / revolution stirrer is preferably 1 minute to 30 minutes, more preferably 5 minutes to 15 minutes, as the total time when switching from the atmospheric atmosphere to the vacuum atmosphere on the way as described above. Can be done. If the stirring time is short, there is a concern that the dispersion of the granular sample 2 in the liquid resin material 3 will be insufficient. On the other hand, if the stirring time is too long, the granular sample 2 in the liquid resin material 3 may be insufficiently dispersed. There is a risk of particle destruction due to the collision of the two particles with each other.

After stirring the granular sample 2 and the liquid resin material 3 in the container 1 using the planetary rotation mixer in this way, the above-mentioned resin is heated to a predetermined temperature, for example, 20 ° C to 60 ° C. Combined with the action of the curing agent, the liquid resin material 3 is cured. Thereby, a sample-embedded resin in which a granular sample is embedded and fixed in the cured resin material can be produced.

Here, if a long time is left from stirring until the liquid resin material 3 is cured, the granular sample 2 settles in the liquid resin material 3 in the container 1 due to the action of gravity, and the dispersibility deteriorates. Is a concern. On the contrary, if the time from stirring to curing the liquid resin material 3 is short, there is a concern that the temperature of the granular sample 2 rises during heating, and in this case, the granular sample 2 may be deteriorated by heat. be. Therefore, the time until the curing of the liquid resin material 3 is completed after stirring with the rotation / revolution stirrer is preferably 30 minutes to 60 minutes, more preferably 30 minutes to 40 minutes.

In the sample-embedded resin prepared as described above, the particle size distribution of the particles of the granular sample dispersed in the resin material in the sample-embedded resin is almost the same as, that is, almost the same as the particle size distribution of the granular sample before embedding. It is preferable that the same tendency is obtained from the viewpoint of suppressing aggregation of particles.
Then, such a sample-embedded resin can be used for analysis of the element content, particle size distribution, elemental separation degree, etc. of the granular sample using various analyzers. In particular, when the particles constituting the granular sample are ore particles, the sample-embedded resin can be effectively used for analysis by a mineral analysis system (Mineral Liberation Analyzer, MLA).

Next, the method for producing the sample-embedded resin for analysis of the present invention was carried out on a trial basis, and its effect was confirmed, which will be described below. However, the description here is for the purpose of mere illustration, and is not intended to be limited thereto.

As shown in Table 1, a method using an ultrasonic stirrer (manual stirring method) and rotation / revolution stirring for each of the coarsely selected ore, the coarsely selected concentrate and the primary selected concentrate as the sample which is a granular sample. A sample-embedded resin was prepared using each of the machine-based methods (mixer stirring method).

In the conventional method, the samples were sieved using a sieve, the under-sieve and the top of the sieve were mixed, and the same amount of the mixed sample and graphite were put into a 1-inch clear cup, and they were mixed manually. Next, the main agent of the epoxy resin (Epocure 2 manufactured by Buehler) and the curing agent are mixed at a ratio of 2: 1 and defoamed with a vacuum desiccator, and then the same amount as the sample is poured into the above clear cup and manually. Mix well in the work. Then, the mixture was stirred with an ultrasonic stirrer for 9 minutes, defoamed with a vacuum desiccator for 10 minutes, the remaining epoxy resin was poured into a clear cup, and then the epoxy resin was cured in the air.

In the mixer stirring method, the sample was put into a clear cup together with the same epoxy resin as above, and then stirred using a rotating revolution agitator (Awatori Rentaro (registered trademark) manufactured by Shinky Co., Ltd.). Then, the epoxy resin was cured in the atmosphere. The stirring conditions at this time are as shown in Table 1. The rotation speed in Table 1 is the rotation speed of the revolution. As other conditions, the rotation speed was set to 1/2 of the revolution speed, and the inclination angle of the rotation axis was set to 45 ° with respect to the revolution axis. The revolution axis was parallel to the vertical direction.

For the sample-embedded resin obtained by each of the above methods, the particle size distribution of the granular sample embedded and fixed in the resin material was measured by MLA, and the particle size of the granular sample before embedding was measured by the particle size distribution meter (Nikki). The results measured by MT3300EX manufactured by Co., Ltd.) are shown in graphs in FIGS. 4 to 6.

In addition, the backscattered electron images and mineral species maps of the sample-embedded resin obtained by the manual stirring method and the mixer stirring method for the coarsely selected ore are shown in FIGS. 7 and 8, respectively, and the manual stirring method and the mixer stirring method for the coarsely selected concentrate are used. The backscattered electron images and mineral species maps of the sample-embedded resin are shown in FIGS. 9 and 10, respectively, and the backscattered electron images and mineral species maps of the sample-embedded resin obtained by the manual stirring method and the mixer stirring method for the primary selected concentrate are shown in FIGS. And 12 show. Here, the backscattered electron image is an image of the backscattered electron intensity, and the mineral species map is a map showing the mineral species by identifying the energy spectrum and the standard mineral spectrum for each mineral. 7 and 9 to 11 show the surface which is one end face of the columnar sample-embedded resin, and FIGS. 8 and 12 show the surface and the axial direction of the columnar sample-embedded resin. It is about the cross section.

From the results shown in FIGS. 4 to 6, it can be seen that the tendency of the granular sample before embedding and the particle size distribution meter is closer to that of the manual stirring method, especially when the vacuum atmosphere is set by the mixer stirring method. Further, in the photographs of the sample-embedded resin by the manual stirring method shown in FIGS. 7, 9 and 11, large agglomeration of particles is confirmed, whereas the sample embedding by the mixer stirring method shown in FIGS. 8, 10 and 12 is confirmed. It is clear from the resin photographs that there is little such agglomeration.
Therefore, according to the present invention, it was found that the agglomeration of the particles of the granular sample in the resin material can be suppressed and the dispersibility of the granular sample in the resin material can be improved.

1 Container 2 Granular sample 3 Liquid resin material 4, 4a Container containing granular sample and liquid resin material θ Tilt angle of the rotation axis with respect to the revolution axis

Claims (8)

A granular sample to be analyzed, which is composed of particles having a non-uniform particle size and contains a plurality of types of simple substances and / or compounds, is embedded in a resin material to prepare a sample-embedded resin in which the granular sample is fixed in the resin material. It ’s a method,
By putting the granular sample together with the liquid resin material into the container and rotating the container containing the granular sample and the liquid resin material in the direction opposite to the rotation while rotating with a rotation / revolution stirrer. After stirring the granular sample and the liquid resin material in the container, the liquid resin material is cured .
A method for producing a sample-embedded resin for analysis , wherein the initial stage of stirring by the rotation / revolution stirrer is performed in an atmospheric atmosphere, and then at least the final stage is performed in a vacuum atmosphere . A granular sample to be analyzed, which is composed of particles having a non-uniform particle size and contains a plurality of types of simple substances and / or compounds, is embedded in a resin material to prepare a sample-embedded resin in which the granular sample is fixed in the resin material. It ’s a method,
The granular sample is put into the container together with the liquid resin material, and the container containing the granular sample and the liquid resin material is rotated in the same rotation direction as the rotation while rotating with a rotation / revolution stirrer. After stirring the granular sample and the liquid resin material inside, the liquid resin material is cured .
A method for producing a sample-embedded resin for analysis , wherein the initial stage of stirring by the rotation / revolution stirrer is performed in an atmospheric atmosphere, and then at least the final stage is performed in a vacuum atmosphere . The method for producing a sample-embedded resin for analysis according to claim 1 or 2, wherein the revolution speed at the time of stirring by a rotation / revolution stirrer is 400 rpm to 2000 rpm. The method for producing a sample-embedded resin for analysis according to any one of claims 1 to 3 , wherein the stirring time by the rotation / revolution stirrer is 1 minute to 30 minutes. The analytical sample-embedded resin according to any one of claims 1 to 4 , wherein the time required to complete the curing of the liquid resin material after stirring by the planetary rotation mixer is 30 to 60 minutes. Manufacturing method. The method for producing a sample-embedded resin for analysis according to any one of claims 1 to 5 , wherein the ratio of the granular sample to the liquid resin material to be charged into the container is 100% by volume to 300% by volume. The method for producing a sample-embedded resin for analysis according to any one of claims 1 to 6 , wherein the particles constituting the granular sample are ore particles. The analytical sample-embedded resin according to any one of claims 1 to 7 , wherein a container in which a plurality of containers containing a granular sample and a liquid resin material are arranged is used as the container to be rotated by a rotation / revolution stirrer. Manufacturing method.

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