JP2019090686A - Method of preparing resin embedded with analysis sample, and resin embedded with analysis sample - Google Patents

Method of preparing resin embedded with analysis sample, and resin embedded with analysis sample Download PDF

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JP2019090686A
JP2019090686A JP2017219424A JP2017219424A JP2019090686A JP 2019090686 A JP2019090686 A JP 2019090686A JP 2017219424 A JP2017219424 A JP 2017219424A JP 2017219424 A JP2017219424 A JP 2017219424A JP 2019090686 A JP2019090686 A JP 2019090686A
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resin
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particles
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JP7018741B2 (en
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昭弘 麻生
Akihiro Aso
昭弘 麻生
木村　昌弘
Masahiro Kimura
昌弘 木村
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JX Nippon Mining and Metals Corp
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Abstract

To provide a method of preparing a resin embedded with an analysis sample, which does not require a heating process, which tends to cause uneven distribution of a granular sample due to sedimentation difference, to cure a liquid resin material mixed with the granular sample, and to provide the resin embedded with an analysis sample.SOLUTION: There is provided a method of preparing a resin embedded with an analysis sample, comprising a granular sample 2 immobilized in a resin material 3, obtained by embedding the target granular sample 2, comprising particles having non-uniform diameters and containing a plurality of types of single molecules and/or compounds, in the resin material 3. The method comprises steps of; mixing a granular sample 2 with a liquid resin material 3 containing an ultraviolet-curable resin; agitating a mixture 4 of the granular sample 2 and the liquid resin material 3; and irradiating the mixture 4 with ultraviolet light to cure the liquid resin material 3 of the mixture 4.SELECTED DRAWING: Figure 1

Description

この発明は、分析の対象とする微小な粒状試料を、分析に先立ち、樹脂材料に埋め込んで固定して、分析用試料埋込樹脂を作製する方法および、分析用試料埋込樹脂に関するものであり、特には、樹脂材料中の粒状試料の偏りを抑制することのできる技術を提案するものである。   The present invention relates to a method for preparing a sample embedding resin for analysis by embedding and fixing a fine particulate sample to be analyzed in a resin material prior to analysis, and a sample embedding resin for analysis. In particular, the present invention proposes a technique capable of suppressing the deviation of the particulate sample in the resin material.

たとえば、鉱石、スラグ、汚泥、粉塵もしくは、電気電子機器等のリサイクル原料その他の不均一な組成および粒径の粒子からなる粒状試料の元素含有量、粒度分布、単体分離度などを計測して分析するに際しては、その粒状試料を構成する粒子が微小であることから、分析装置にセットする前に、当該粒状試料を樹脂材料に埋め込んで固定して、試料埋込樹脂を得ることが一般に行われている。なお、このような分析装置の一例として、鉱物解析システム（Ｍｉｎｅｒａｌ Ｌｉｂｅｒａｔｉｏｎ Ａｎａｌｙｚｅｒ、ＭＬＡ）は、ＳＥＭ−ＥＤＳをベースとして鉱石粒子の解析を行うものであり、特に鉱物資源の分野で用いられている。   For example, measure and analyze the elemental content, particle size distribution, single substance separation degree, etc. of granular samples consisting of particles of non-uniform composition and particle size such as ore, slag, sludge, dust or recycled raw materials such as electric and electronic equipment Because the particles that make up the particulate sample are so small, it is common practice to embed and fix the particulate sample in a resin material to obtain a sample-embedded resin before setting it in the analyzer. ing. As an example of such an analyzer, a mineral analysis system (Mineral Liberation Analyzer, MLA) analyzes ore particles based on SEM-EDS, and is used particularly in the field of mineral resources.

かかる試料埋込樹脂では、分析精度を高めるため、粒状試料が樹脂材料中に十分均一に分布した状態で固定することが求められる。
それゆえに従来は、試料埋込樹脂を作製する場合、はじめに、粒状試料を、熱硬化性樹脂であるエポキシ樹脂からなる液体状樹脂材料と混合させ、それにより得られる混合物に対して、手作業によるかき混ぜや、超音波撹拌機での容器内の攪拌等を十分に行った後、該混合物を大気中で加熱し、そこに含まれる液体状樹脂材料を硬化させることとしていた。 In such a sample-embedded resin, in order to improve analysis accuracy, it is required that the particulate sample be fixed in a sufficiently uniformly distributed state in the resin material.
Therefore, conventionally, when producing a sample embedding resin, first, a particulate sample is mixed with a liquid resin material made of an epoxy resin which is a thermosetting resin, and the resulting mixture is manually processed. After sufficiently performing stirring, stirring in a container with an ultrasonic stirrer, or the like, the mixture is heated in the air to cure the liquid resin material contained therein.

しかしながら、上述したようにして、混合物の攪拌を行ったとしても、その後にエポキシ樹脂等の熱硬化性の液体状樹脂材料を加熱することで硬化させる場合は、加熱開始から液体状樹脂材料の昇温を経て液体状樹脂材料の硬化が完了するまで比較的長い時間を要することから、その硬化の完了までの間に、液体状樹脂材料中の粒状試料のうち、重量の軽い粒子は上方側に浮上する一方で、重量の重い粒子は下方側に沈降して、樹脂材料中の粒状試料に偏りが生じる。特に、分析の測定面となることがある下方側には、重量の重い粒子が多く存在することになり、そのような試料埋込樹脂を用いて粒子の分析や解析を行うと、その測定面が当該粒状試料を代表するものではないことに起因して、所期した分析ないし解析の結果が得られないという問題がある。   However, even if the mixture is stirred as described above, if the thermosetting liquid resin material such as an epoxy resin is cured by heating thereafter, the rise of the liquid resin material from the start of heating Since it takes a relatively long time to complete curing of the liquid resin material through heating, the light weight particles of the particulate sample in the liquid resin material are directed upward during the completion of the curing. While floating, heavy particles settle downward and cause a deviation in the granular sample in the resin material. In particular, on the lower side, which may be the measurement surface of analysis, many heavy particles are present, and when analysis and analysis of particles are performed using such a sample embedding resin, the measurement surface There is a problem that the result of the intended analysis or analysis can not be obtained because the particle is not representative of the particulate sample.

なお、この種の問題に関して、特許文献１には、「粒状試料が樹脂に包埋されてなる樹脂包埋試料の作製方法であって、前記粒状試料と粒状のペレット用樹脂との混合物を固形化して、ペレット成形体を得る固形化工程と、前記ペレット成形体に含まれる前記ペレット用樹脂を溶融固化させて、固化ペレットを得る溶融固化工程と、を有することを特徴とする樹脂包埋試料の作製方法」が提案されている。そして、この方法によれば、「試料作製時に、試料に含まれる鉱石粒子の比重差に起因する鉱物の存在状態の偏りを生じさせず、かつ分析試料数が増える等の分析時の負担を軽減できる樹脂包埋試料およびその作製方法を提供することができる」とされている。   In addition, regarding this kind of problem, Patent Document 1 states that “a method for producing a resin-embedded sample in which a granular sample is embedded in a resin, and a mixture of the granular sample and a resin for pelletizing is solidified. Resin-embedded sample comprising: a solidification step to obtain a pellet molded body, and a melt-solidification step to melt and solidify the resin for pellet contained in the pellet molded body to obtain solidified pellets "Production method of" has been proposed. And, according to this method, “the load of analysis such as increase in the number of analysis samples is reduced, without causing the bias of the existence state of minerals due to the specific gravity difference of the ore particles contained in the sample at the time of sample preparation” It can be said that it can provide a resin-embedded sample that can be

また特許文献２には、「分析対象である粒状試料、熱硬化性樹脂および固形潤滑剤を含む試料含有材料を固形化し、ペレット成形体を形成する固形化工程と、前記ペレット成形体を加熱し、前記熱硬化性樹脂を溶融固化させることにより、前記粒状試料および前記固形潤滑剤が前記熱硬化性樹脂に包埋されて構成される固化ペレットを形成する溶融固化工程と、を有することを特徴とする、樹脂包埋試料の作製方法」が記載されており、これによると、「粒状試料の比重差に起因する存在状態の偏りが小さく、かつ取り扱うのに十分な強度を有する樹脂包埋試料が得られる」とされている。   Further, in Patent Document 2, “A solidifying step of solidifying a sample containing material to be analyzed including a particulate sample, a thermosetting resin and a solid lubricant to form a pellet molded body, and heating the pellet molded body And a solidifying step of forming solidified pellets constituted by embedding the particulate sample and the solid lubricant in the thermosetting resin by melting and solidifying the thermosetting resin. The method for preparing a resin-embedded sample according to the present invention is described. According to this, a resin-embedded sample having a small deviation of the existing state due to the specific gravity difference of the granular sample and having sufficient strength for handling Is said to be

特開２０１６−５０９１８号公報JP, 2016-50918, A 特開２０１７−６２２２３号公報JP, 2017-62223, A

特許文献１及び２では、液体状樹脂材料に代えて粒状樹脂材料を用いることとしているが、この場合、粒状試料を粒状樹脂の間に偏りなく均等に存在するよう混ぜることは容易ではなく、さらに凝集がなくならない。それにより、特許文献１及び２に記載された方法によっては、樹脂材料中に粒状試料が均一に分布した試料埋込樹脂を確実に作製できるとは言い難い。   In Patent Documents 1 and 2, instead of the liquid resin material, a granular resin material is used, but in this case, it is not easy to mix the granular samples so as to be evenly and evenly between the granular resins. Aggregation does not disappear. Thus, it is difficult to say that the method described in Patent Documents 1 and 2 can reliably produce a sample embedding resin in which granular samples are uniformly distributed in a resin material.

この発明は、従来技術が抱えるこのような問題を解決することを課題とするものであり、その目的は、粒状試料と混合させた液体状樹脂材料を硬化させるに当り、粒状試料の沈降差による不均一な分布を招く加熱処理を行う必要のない分析用試料埋込樹脂の作製方法および、分析用試料埋込樹脂を提供することにある。   The present invention has an object to solve such problems in the prior art, and the purpose thereof is to set the difference in sedimentation of the granular sample when curing the liquid resin material mixed with the granular sample. It is an object of the present invention to provide a method for producing a sample embedding resin for analysis which does not require heat treatment which leads to uneven distribution, and a sample embedding resin for analysis.

発明者は鋭意検討の結果、試料埋込樹脂を作製する際に、これまでに用いていたエポキシ樹脂等の熱硬化性の液体状樹脂材料を、紫外線硬化樹脂を含む液体状樹脂材料とすることにより、攪拌後の紫外線の照射で比較的短い時間で、当該液体状樹脂材料を硬化できることを見出した。この場合、液体状樹脂材料の硬化のための加熱処理が不要になるとともに、樹脂材料中の粒状試料の不均一な分布を抑制することができる。   As a result of intensive investigations, the inventor of the present invention should use a thermosetting liquid resin material such as an epoxy resin, which has been used until now, as a liquid resin material containing an ultraviolet curing resin when producing a sample embedding resin. It has been found that the liquid resin material can be cured in a relatively short time by irradiation of ultraviolet light after stirring. In this case, heat treatment for curing the liquid resin material is not necessary, and nonuniform distribution of the granular sample in the resin material can be suppressed.

この知見の下、この発明の分析用試料埋込樹脂の作製方法は、粒径が不均一な粒子からなり複数種類の単体及び／又は化合物を含む分析対象の粒状試料を、樹脂材料に埋め込んで、該樹脂材料中に前記粒状試料を固定した試料埋込樹脂を作製する方法であって、前記粒状試料を、紫外線硬化樹脂を含む液体状樹脂材料と混合させ、粒状試料と液体状樹脂材料との混合物を攪拌し、その後、前記混合物に紫外線を照射して該混合物中の液体状樹脂材料を硬化させることにある。   Under this finding, the method for producing a sample embedding resin for analysis according to the present invention embeds a particulate sample to be analyzed which is composed of particles having nonuniform particle sizes and which contains plural kinds of single substances and / or compounds in a resin material. A method for producing a sample embedding resin in which the particulate sample is fixed in the resin material, wherein the particulate sample is mixed with a liquid resin material containing an ultraviolet curable resin, and the particulate sample and the liquid resin material The mixture is stirred, and then the mixture is irradiated with ultraviolet light to cure the liquid resin material in the mixture.

この発明の分析用試料埋込樹脂の作製方法では、前記紫外線硬化樹脂をアクリル樹脂とすることが好ましい。   In the method of producing a sample embedding resin for analysis of the present invention, the ultraviolet curable resin is preferably an acrylic resin.

またこの発明の分析用試料埋込樹脂の作製方法では、液体状樹脂材料を硬化させる際に、前記混合物の周囲に隈なく紫外線を照射することが好ましい。
特にこの場合は、液体状樹脂材料を硬化させる際に、前記混合物の周囲に全方向から同時に紫外線を照射することがより一層好ましい。 Further, in the method for producing a sample embedding resin for analysis of the present invention, it is preferable that the periphery of the mixture is irradiated with ultraviolet rays when curing the liquid resin material.
In this case, in particular, it is more preferable to irradiate ultraviolet light from all directions simultaneously around the mixture when curing the liquid resin material.

この発明の分析用試料埋込樹脂の作製方法では、前記混合物に照射する紫外線の照度を、２００００ｍＷ／ｃｍ2〜３６０００ｍＷ／ｃｍ2とすることが好ましい。
また、この発明の分析用試料埋込樹脂の作製方法では、前記混合物への紫外線の照射時間を、１分〜１０分とすることが好ましい。 In the method of producing a sample embedding resin for analysis of the present invention, it is preferable that the illuminance of the ultraviolet light irradiated to the mixture be 20000 mW / cm 2 to 36000 mW / cm 2 .
Further, in the method of preparing a sample embedding resin for analysis of the present invention, the irradiation time of the ultraviolet light to the mixture is preferably set to 1 minute to 10 minutes.

この発明の分析用試料埋込樹脂の作製方法では、前記混合物の攪拌後、液体状樹脂材料の硬化が完了するまでの時間を、１分〜１０分、さらに１分〜５分とすることが好適である。   In the method for producing a sample embedding resin for analysis of the present invention, after stirring the mixture, the time until the curing of the liquid resin material is completed may be 1 minute to 10 minutes, and further 1 minute to 5 minutes. It is suitable.

なお、この発明の分析用試料埋込樹脂の作製方法では、前記粒状試料を構成する粒子を鉱石粒子とすることが好ましい。   In the method for producing a sample embedding resin for analysis of the present invention, it is preferable that the particles constituting the particulate sample be ore particles.

この発明の分析用試料埋込樹脂は、粒径が不均一な粒子からなり複数種類の化合物を含む分析対象の粒状試料と、前記粒状試料が埋め込まれた樹脂材料とを有し、前記樹脂材料が紫外線硬化樹脂を含むものである。   The sample embedding resin for analysis of the present invention comprises a particulate sample to be analyzed which is composed of particles having nonuniform particle sizes and which contains a plurality of types of compounds, and a resin material in which the particulate sample is embedded, Is an ultraviolet curable resin.

この発明の分析用試料埋込樹脂では、前記紫外線硬化樹脂がアクリル樹脂であることが好ましい。
なお、この発明の分析用試料埋込樹脂では、前記粒状試料を構成する粒子が鉱石粒子であることが好ましい。 In the sample embedding resin for analysis of the present invention, the ultraviolet curing resin is preferably an acrylic resin.
In addition, in the sample embedding resin for analysis of the present invention, it is preferable that particles constituting the particulate sample are ore particles.

この発明によれば、前記粒状試料を、紫外線硬化樹脂を含む液体状樹脂材料と混合させ、その混合物を攪拌した後、混合物に紫外線を照射することにより、粒状試料の沈降による不均一な分布を招く加熱処理を行うことなしに、混合物中の液体状樹脂材料を硬化させることができる。   According to the present invention, the particulate sample is mixed with the liquid resin material containing the ultraviolet curing resin, and after stirring the mixture, the mixture is irradiated with ultraviolet rays, thereby causing uneven distribution due to sedimentation of the particulate sample. The liquid resin material in the mixture can be cured without conducting the heat treatment.

この発明の一の実施形態に係る分析用試料埋込樹脂の作製方法を実施する際の粒状試料を液体状樹脂材料と混合させた状態を模式的に示す斜視図である。It is a perspective view which shows typically the state which mixed the granular sample at the time of enforcing the manufacturing method of sample embedding resin for analysis which concerns on one Embodiment of this invention with a liquid resin material.

以下に、この発明の実施の形態について詳細に説明する。
この発明の一の実施形態に係る分析用試料埋込樹脂の作製方法は、粒径が不均一な粒子からなり複数種類の単体及び／又は化合物を含む分析対象の粒状試料を、樹脂材料に埋め込んで、該樹脂材料中に前記粒状試料を固定した試料埋込樹脂を作製するものであり、図１に例示するように、たとえば底付き円筒状等の容器１を用いて、該容器１内で、粒状試料２を、紫外線硬化樹脂を含む液体状樹脂材料３と混合させ、粒状試料２と液体状樹脂材料３との混合物４を攪拌し、その後、混合物４に紫外線を照射して混合物４中の液体状樹脂材料３を硬化させる。 Hereinafter, embodiments of the present invention will be described in detail.
According to one embodiment of the present invention, there is provided a method of preparing a sample embedding resin for analysis according to the present invention, in which a particulate sample to be analyzed consisting of particles having nonuniform particle sizes and containing plural kinds of single substances and / or compounds is embedded in a resin material. Then, a sample-embedded resin in which the granular sample is fixed in the resin material is manufactured, and as illustrated in FIG. 1, for example, using a container 1 such as a bottomed cylindrical shape in the container 1. The granular sample 2 is mixed with the liquid resin material 3 containing the ultraviolet curing resin, the mixture 4 of the granular sample 2 and the liquid resin material 3 is stirred, and then the mixture 4 is irradiated with ultraviolet light to be in the mixture 4 The liquid resin material 3 is cured.

（粒状試料）
分析の対象とする粒状試料２は、鉱石、スラグ、汚泥、粉塵もしくは、電気電子機器を含むそのリサイクル原料等に対して所定の処理を施すこと等によって、比較的小さい粒子となったものとすることができる。このような粒状試料２は通常、組成および粒径の意図的な均一化が行われていないので、複数種類の化合物を含むとともに、粒径が均一ではなくばらついた粒子からなる。 (Granular sample)
The granular sample 2 to be analyzed shall be relatively small particles by subjecting ore, slag, sludge, dust or its recycled materials including electric and electronic equipment to predetermined treatment etc. be able to. Since such granular sample 2 usually does not have intentional homogenization of composition and particle size, it contains particles of a plurality of types of particles and is not uniform in particle size as well as containing various types of compounds.

なかでも、鉱石粒子からなる粒状試料を対象とする場合、このような鉱石粒子は銅鉱石を含むことがあり、これには、たとえば、輝銅鉱、銅藍、黄銅鉱、班銅鉱、硫砒銅鉱、ブロシャン銅鉱等が含まれ得る。銅鉱石以外にも黄鉄鉱、磁鉄鉱、ケイ酸塩鉱物、輝水鉛鉱、金粒子等も含まれ得る。なおケイ酸塩鉱物としては、正長石、曹長石、斜長石、白雲母、黒雲母、石英等がある。   Among them, when targeting granular samples consisting of ore particles, such ore particles may include copper ore, and examples of such ore particles include copper ore, copper ore, chalcopyrite, copper ore, arsenopyrite, etc. Broshan copper ore may be included. Besides copper ore, pyrite, magnetite, silicate mineral, molybdenite, gold particles and the like may be included. Examples of silicate minerals include orthoclase, albite, plagioclase, muscovite, biotite and quartz.

スラグからなる粒状試料を対象とする場合、スラグ自体がＳｉＯ2、ＣａＯ、Ａｌ2Ｏ3、ＦｅＯ及びＦｅ3Ｏ4等を含む複雑な組成を持ち、さらにスラグ中にマット粒子やメタル粒子を含む場合がある。
電気電子機器からなる粒状試料の場合、基板に含まれる樹脂部や回路を構成する金属部、難燃剤部等の様々な組成を持つ粒子が存在する。
汚泥、粉塵に至っては単一の組成となっている場合はまず無い。 When targeting granular samples made of slag, the slag itself has a complicated composition including SiO 2 , CaO, Al 2 O 3 , FeO, Fe 3 O 4 and the like, and further contains matte particles and metal particles in the slag. There is a case.
In the case of a granular sample composed of an electric and electronic device, particles having various compositions such as a resin part contained in a substrate, a metal part constituting a circuit, and a flame retardant part are present.
In the case of sludge and dust, it is unlikely that they have a single composition.

粒状試料を構成する粒子の粒径は、たとえば１μｍ〜７００μｍ、典型的には２０μｍ〜２００μｍの範囲で、比較的全体的に分布していて不均一である。なお、粒度分布計で測定できる粒度は、たとえば０．２４３μｍ〜２０００μｍである場合があるが、上述したような粒状試料の粒径はこの範囲で不均一に分布している。   The particle size of the particles constituting the particulate sample is relatively uniformly distributed and nonuniform, for example, in the range of 1 μm to 700 μm, typically 20 μm to 200 μm. In addition, although the particle size which can be measured with a particle size distribution analyzer may be 0.243 micrometers-2000 micrometers, for example, the particle size of the above-mentioned granular sample is distributed unevenly in this range.

（樹脂材料）
この発明の実施形態では、上述した粒状試料２を埋め込んで固定するための樹脂材料３は、後述するように粒状試料２と混合させる際および攪拌の際に液体状に維持できるものであって、紫外線の照射により硬化する紫外線硬化樹脂を含むものとする。このような紫外線硬化樹脂を含む樹脂材料３を用いることにより、液体の状態のものに紫外線を照射すると比較的瞬時に硬化することから、液体状樹脂材料３を硬化させる際に、粒状試料２の沈降が生じやすい加熱処理を施すことが不要になる。それにより、粒状試料２の各粒子の沈降差に起因する試料埋込樹脂における粒状試料２の不均一な分布を抑制することができる。 (Resin material)
In the embodiment of the present invention, the resin material 3 for embedding and fixing the above-described granular sample 2 can be maintained in a liquid state when it is mixed with the granular sample 2 as described later, and during stirring. It includes an ultraviolet curable resin which is cured by irradiation of ultraviolet light. By using the resin material 3 containing such an ultraviolet curable resin, the liquid state is cured relatively quickly when ultraviolet rays are irradiated, so when the liquid resin material 3 is cured, the granular sample 2 is obtained. It becomes unnecessary to perform the heat treatment which tends to cause sedimentation. Thereby, it is possible to suppress the non-uniform distribution of the particulate sample 2 in the sample embedding resin caused by the difference in sedimentation of the particles of the particulate sample 2.

紫外線硬化樹脂としては、アクリル樹脂、ウレタン樹脂、ウレタンアクリレート樹脂、ビニルエステル樹脂、ポリエステル・アルキド樹脂、ＵＶエポキシ樹脂、エポキシアクリレート樹脂等を挙げることができる。なかでも、アクリル樹脂は、ＭＬＡ等による分析の際に照射され得る電子線に対して十分な強度を有することから、試料埋込樹脂の樹脂材料３として特に有効に用いることができる。
このような紫外線硬化樹脂は市販されており、当該市販品を用いることが可能である。 Examples of UV curable resins include acrylic resins, urethane resins, urethane acrylate resins, vinyl ester resins, polyester alkyd resins, UV epoxy resins, epoxy acrylate resins and the like. Among them, the acrylic resin is particularly effective as the resin material 3 of the sample embedding resin because it has sufficient strength to the electron beam that can be irradiated at the time of analysis by MLA or the like.
Such UV curable resin is commercially available, and it is possible to use the commercially available product.

（分析用試料埋込樹脂の作製方法）
上記の粒状試料および樹脂材料にて分析用の試料埋込樹脂を作製するには、はじめに、図１に示すように所定の透明な容器１に、粒状試料２を、紫外線硬化樹脂を含む液体状樹脂材料３とともに投入して、粒状試料２を液体状樹脂材料３と混合させ、粒状試料２と液体状樹脂材料３との混合物４を得る。なおこれに先立って、粒状試料２を所定の篩を用いて篩分けした後、篩上と篩下を混ぜ合わせる篩別処理その他の所要の処理を行ってもよい。またここでは、粒状試料２に、後述の攪拌時に粒子の凝集を除去して粒子どうしを分離させるべく機能するグラファイト等の粒状の固形物を混合させてもよい。 (Preparation method of sample embedding resin for analysis)
In order to produce a sample-embedded resin for analysis using the above-mentioned granular sample and resin material, first, as shown in FIG. 1, a liquid sample containing a UV-curable resin and a granular sample 2 in a predetermined transparent container 1 Then, the granular sample 2 is mixed with the liquid resin material 3 in order to obtain a mixture 4 of the granular sample 2 and the liquid resin material 3. Prior to this, the particulate sample 2 may be sieved using a predetermined sieve, and then the sieved treatment and other required treatments may be carried out by combining the sieve on the sieve and the sieve. Here, the granular sample 2 may be mixed with a granular solid such as graphite which functions to separate particles by removing aggregation of particles during stirring described later.

次いで、手作業及び／又は超音波撹拌機により容器１内の混合物４を攪拌し、粒状試料２の粒子どうしの凝集をなくして、粒子を十分に分散させる。これにより、作製される試料埋込樹脂の粒状試料２の分散性を高めることができる。
なお、この攪拌前や攪拌後に、必要に応じて、真空デシケーター等を用いて、容器１内の液体状樹脂材料中に存在し得る泡を取り除くことができる。また、液体状樹脂材料３を、容器１に投入する前に脱泡しておくことも可能である。 Next, the mixture 4 in the container 1 is stirred by a manual operation and / or an ultrasonic stirrer to eliminate the agglomeration of the particles of the granular sample 2 and to disperse the particles sufficiently. Thereby, the dispersibility of granular sample 2 of sample embedding resin produced can be improved.
Before and after this stirring, if necessary, a vacuum desiccator or the like can be used to remove bubbles that may be present in the liquid resin material in the container 1. It is also possible to degas the liquid resin material 3 before charging it into the container 1.

そして、上記の攪拌の後、容器１内の混合物４に紫外線を照射し、混合物４中の液体状樹脂材料３を硬化させる。
ここでは、たとえば、透明な容器１の外側で、前方に紫外線を発する紫外線照射器を移動させながら、混合物４の周囲に隈なく紫外線を照射することが好ましい。あるいは、粒状試料２を撹拌しながら混合物４の表面に紫外線を照射させることもできる。つまり、紫外線照射による液体状樹脂材料３の硬化時に攪拌してもよい。このときの攪拌には、超音波撹拌機または自転公転撹拌機等を用いてもよい。この場合、混合物４の紫外線に照射される部分が撹拌により常に変化するので、混合物４に隈なく紫外線を当てることができる。あるいは、内部に、混合物４入りの容器１を収容配置可能な紫外線照射器を用いることもでき、この場合、その紫外線照射器の内部で、混合物の周囲に全方向から同時に紫外線を照射することができる。容器１内の、液体状樹脂材料３の粒状試料２で紫外線が遮られる部分にも十分に紫外線を当てることができて、その硬化がより有効に促進される。 And after said stirring, the ultraviolet-ray is irradiated to the mixture 4 in the container 1, and the liquid resin material 3 in the mixture 4 is hardened.
Here, for example, it is preferable to radiate the ultraviolet light around the mixture 4 while moving the ultraviolet irradiator emitting the ultraviolet light forward on the outside of the transparent container 1. Alternatively, the surface of the mixture 4 can be irradiated with ultraviolet light while stirring the particulate sample 2. That is, it may be stirred at the time of curing of the liquid resin material 3 by ultraviolet irradiation. For stirring at this time, an ultrasonic stirrer or a rotation-revolution stirrer may be used. In this case, since the portion of the mixture 4 to be irradiated with ultraviolet light is constantly changed by the stirring, the mixture 4 can be irradiated with ultraviolet light all at once. Alternatively, it is also possible to use an ultraviolet irradiator capable of accommodating and disposing the container 1 containing the mixture 4 therein, in which case the ultraviolet light is irradiated simultaneously from all directions around the mixture inside the ultraviolet irradiator. it can. Ultraviolet rays can be sufficiently applied to the part of the container 1 where the granular sample 2 of the liquid resin material 3 blocks ultraviolet rays, and the curing thereof is more effectively promoted.

なお、ここでいう紫外線は、波長が２００ｎｍ〜４００ｎｍの範囲、典型的には３６５、３８５、４０５ｎｍの範囲にある電磁波を意味する。   In addition, the ultraviolet-ray here means the electromagnetic waves whose wavelength is in the range of 200 nm-400 nm, and typically in the range of 365, 385, and 405 nm.

ここにおいて、混合物４に照射する紫外線の照度は、２００００ｍＷ／ｃｍ2〜３６０００ｍＷ／ｃｍ2とすることが好適である。紫外線の照度が低すぎると、液体状樹脂材料３の硬化に時間がかかり、その際に粒状試料２が沈降することによる粒状試料２の偏りの発生が懸念される。一方、紫外線の照度が高すぎると、ラジカル重合反応が促進され、高熱になり、火災の原因となる可能性がある。このような観点から、混合物４に照射する紫外線の照度は、２００００ｍＷ／ｃｍ2〜３６０００ｍＷ／ｃｍ2とすることが好ましい。 Here, it is preferable that the illuminance of the ultraviolet light applied to the mixture 4 be 20000 mW / cm 2 to 36000 mW / cm 2 . If the illuminance of the ultraviolet light is too low, it takes time to cure the liquid resin material 3, and at that time, the occurrence of the deviation of the granular sample 2 due to the sedimentation of the granular sample 2 is concerned. On the other hand, if the illuminance of the ultraviolet light is too high, the radical polymerization reaction is promoted, resulting in high heat, which may cause a fire. From such a viewpoint, it is preferable that the illuminance of the ultraviolet light irradiated to the mixture 4 be 20000 mW / cm 2 to 36000 mW / cm 2 .

またここで、混合物へ紫外線を照射する時間は、好ましくは１分〜１０分、より好ましくは２分〜３分とする。紫外線の照射時間が短すぎる場合は、液体状樹脂材料３の硬化が不十分となって、その後の分析に支障をきたすおそれがある。紫外線の照射時間が長すぎる場合は、粒状試料２の沈降差による粒状試料２の不均一な分布の問題が生じる可能性がある。   Here, the time for irradiating the mixture with ultraviolet light is preferably 1 minute to 10 minutes, more preferably 2 minutes to 3 minutes. If the irradiation time of the ultraviolet light is too short, the curing of the liquid resin material 3 may be insufficient, which may affect the subsequent analysis. If the irradiation time of the ultraviolet light is too long, the problem of non-uniform distribution of the granular sample 2 due to the sedimentation difference of the granular sample 2 may occur.

また、攪拌後に、紫外線を照射して液体状樹脂材料３の硬化が完了するまでの時間が長いと、この間に粒状試料２が沈降して粒状試料２の存在状態に偏りが生じることが懸念される。それ故に、攪拌が終了した時点から液体状樹脂材料３の硬化が完了するまでの時間は、１分〜１０分とすることが好ましく、さらに２分〜３分とすることが一層好ましい。
なお、液体状樹脂材料３の硬化が完了したかどうかは、つまようじ等で押して、凹まないことにより確認する。 In addition, there is a concern that if the time to complete the curing of the liquid resin material 3 is long after irradiation with ultraviolet light after the stirring, the granular sample 2 will settle and the presence of the granular sample 2 will be biased. Ru. Therefore, the time from completion of the stirring to completion of curing of the liquid resin material 3 is preferably 1 minute to 10 minutes, and more preferably 2 minutes to 3 minutes.
In addition, it is confirmed by pushing with a toothpick etc. and not denting whether hardening of the liquid resin material 3 was completed.

このようにして紫外線を照射することで液体状樹脂材料３を硬化させて、試料埋込樹脂を作製することができる。したがって、この実施形態では、液体状樹脂材料３の硬化のために、加熱処理を行うことを要しない。それにより、加熱処理時に生じ得る粒状試料２の沈降を防止することができる。   In this manner, the liquid resin material 3 can be cured by irradiating ultraviolet light to produce a sample embedding resin. Therefore, in this embodiment, it is not necessary to perform a heat treatment for curing the liquid resin material 3. Thereby, sedimentation of the particulate sample 2 which may occur at the time of heat treatment can be prevented.

この試料埋込樹脂は、粒径が不均一な粒子からなり複数種類の化合物を含む分析対象の粒状試料２と、前記粒状試料２が埋め込まれた樹脂材料３とを有するものであり、樹脂材料３には、アクリル樹脂等の先述した紫外線硬化樹脂が含まれる。   The sample-embedded resin comprises a particulate sample 2 to be analyzed which is composed of particles having nonuniform particle sizes and contains a plurality of types of compounds, and a resin material 3 in which the particulate sample 2 is embedded. 3 includes the above-described ultraviolet curable resin such as an acrylic resin.

かかる試料埋込樹脂は、試料埋込樹脂における樹脂材料３中に分散した粒状試料２の粒子の粒度分布が、埋め込み前の粒状試料２の粒度分布とほぼ同一、つまりほぼ同様の傾向となっていることが、粒子どうしの凝集抑制の観点から好適である。
そして、このような試料埋込樹脂は、様々な分析装置を用いた粒状試料２の元素含有量、粒度分布、単体分離度などの分析に供することができる。特にここで、粒状試料２を構成する粒子を鉱石粒子とした場合、その試料埋込樹脂は、鉱物解析システム（Ｍｉｎｅｒａｌ Ｌｉｂｅｒａｔｉｏｎ Ａｎａｌｙｚｅｒ、ＭＬＡ）による分析に有効に用いることができる。 In the sample embedding resin, the particle size distribution of the particles of the granular sample 2 dispersed in the resin material 3 in the sample embedding resin has a tendency substantially the same as the particle size distribution of the granular sample 2 before embedding, that is, almost the same tendency Is preferable from the viewpoint of suppressing aggregation of particles.
And such a sample embedding resin can be provided to analysis of the element content, the particle size distribution, the degree of single substance separation, etc. of the granular sample 2 using various analyzers. In particular, here, when particles constituting the particulate sample 2 are ore particles, the sample embedding resin can be effectively used for analysis by a mineral analysis system (Mineral Liberation Analyzer, MLA).

１ 容器
２ 粒状試料
３ 液体状樹脂材料（樹脂材料）
４ 混合物 1 container 2 granular sample 3 liquid resin material (resin material)
4 mixture

Claims (11)

粒径が不均一な粒子からなり複数種類の単体及び／又は化合物を含む分析対象の粒状試料を、樹脂材料に埋め込んで、該樹脂材料中に前記粒状試料を固定した試料埋込樹脂を作製する方法であって、
前記粒状試料を、紫外線硬化樹脂を含む液体状樹脂材料と混合させ、粒状試料と液体状樹脂材料との混合物を攪拌し、その後、前記混合物に紫外線を照射して該混合物中の液体状樹脂材料を硬化させる、分析用試料埋込樹脂の作製方法。 A particulate sample to be analyzed which is composed of particles having nonuniform particle sizes and which contains plural kinds of single particles and / or compounds is embedded in a resin material to prepare a sample embedding resin in which the particulate sample is fixed in the resin material. Method,
The particulate sample is mixed with a liquid resin material containing an ultraviolet curable resin, the mixture of the particulate sample and the liquid resin material is stirred, and then the mixture is irradiated with ultraviolet light to be a liquid resin material in the mixture. A method of preparing a sample embedding resin for analysis, which cures 前記紫外線硬化樹脂をアクリル樹脂とする、請求項１に記載の分析用試料埋込樹脂の作製方法。   The method for producing a sample embedding resin for analysis according to claim 1, wherein the ultraviolet curing resin is an acrylic resin. 液体状樹脂材料を硬化させる際に、前記混合物の周囲に隈なく紫外線を照射する、請求項１または２に記載の分析用試料埋込樹脂の作製方法。   The method for producing a sample embedding resin for analysis according to claim 1 or 2, wherein ultraviolet light is irradiated to the periphery of the mixture completely when curing the liquid resin material. 液体状樹脂材料を硬化させる際に、前記混合物の周囲に全方向から同時に紫外線を照射する、請求項３に記載の分析用試料埋込樹脂の作製方法。   The method for producing a sample embedding resin for analysis according to claim 3, wherein ultraviolet rays are irradiated simultaneously from all directions around the mixture when curing the liquid resin material. 前記混合物に照射する紫外線の照度を、２００００ｍＷ／ｃｍ2〜３６０００ｍＷ／ｃｍ2とする、請求項１〜４のいずれか一項に記載の分析用試料埋込樹脂の作製方法。 The illuminance of the irradiated ultraviolet ray to the mixture, and 20000mW / cm 2 ~36000mW / cm 2 , a method for manufacturing a sample embedded resin for analysis according to any one of claims 1-4. 前記混合物への紫外線の照射時間を、１分〜１０分とする、請求項１〜５のいずれか一項に記載の分析用試料埋込樹脂の作製方法。   The preparation method of the sample embedding resin for analysis as described in any one of Claims 1-5 which makes irradiation time of the ultraviolet-ray to the said mixture 1 minute-10 minutes. 前記混合物の攪拌後、液体状樹脂材料の硬化が完了するまでの時間を、１分〜１０分とする、請求項１〜６のいずれか一項に記載の分析用試料埋込樹脂の作製方法。   The method for producing a sample embedding resin for analysis according to any one of claims 1 to 6, wherein a time for completing curing of the liquid resin material is set to 1 minute to 10 minutes after stirring the mixture. . 前記粒状試料を構成する粒子を鉱石粒子とする、請求項１〜７のいずれか一項に記載の分析用試料埋込樹脂の作製方法。   The method for producing a sample embedding resin for analysis according to any one of claims 1 to 7, wherein particles constituting the particulate sample are ore particles. 粒径が不均一な粒子からなり複数種類の化合物を含む分析対象の粒状試料と、前記粒状試料が埋め込まれた樹脂材料とを有し、前記樹脂材料が紫外線硬化樹脂を含む分析用試料埋込樹脂。   A particulate sample to be analyzed which is composed of particles having nonuniform particle sizes and which contains a plurality of kinds of compounds, and a resin material in which the particulate sample is embedded, and the resin material contains an ultraviolet curing resin. resin. 前記紫外線硬化樹脂がアクリル樹脂である請求項９に記載の分析用試料埋込樹脂。   The sample embedding resin for analysis according to claim 9, wherein the ultraviolet curing resin is an acrylic resin. 前記粒状試料を構成する粒子が鉱石粒子である請求項９又は１０に記載の分析用試料埋込樹脂。   11. The analytical sample embedding resin according to claim 9, wherein the particles constituting the particulate sample are ore particles.
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