JP6776917B2 - Method of analyzing elemental sulfur distribution - Google Patents
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims description 69
- 238000009826 distribution Methods 0.000 title claims description 31
- 238000000034 method Methods 0.000 title claims description 13
- 239000000523 sample Substances 0.000 claims description 48
- 238000010894 electron beam technology Methods 0.000 claims description 37
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- 230000001678 irradiating effect Effects 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 8
- 238000005211 surface analysis Methods 0.000 description 8
- 230000008022 sublimation Effects 0.000 description 6
- 238000000859 sublimation Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Description
本発明は、単体硫黄分布の分析方法に関する。 The present invention relates to a method for analyzing elemental sulfur distribution.
硫黄を使用する工業製品の製造工程において、硫黄は元素単体で存在する場合や、酸化されて硫黄酸化物で存在する場合がある。単体硫黄は活性の高い多孔質樹脂等に吸着することがあり、こういった試料中の単体硫黄の存在分布を把握することが重要となる。元素の分布を分析する方法としては、例えば、試料を真空中で電子線を照射し発生する特性Ｘ線を測定することにより含有元素の特定や分布の把握を行う電子線マイクロアナライザ（ＥＰＭＡ）がある。ＥＰＭＡは、化学分析の様なバルク（試料全体）の元素を把握するのとは異なり、微小領域で元素がどのように分布しているかを把握することができる（例えば、特許文献１を参照）。 In the manufacturing process of industrial products using sulfur, sulfur may exist as an element alone or may be oxidized and exist as a sulfur oxide. Elemental sulfur may be adsorbed on highly active porous resins and the like, and it is important to understand the distribution of elemental sulfur in such samples. As a method for analyzing the distribution of elements, for example, an electron probe microanalyzer (EPMA) that identifies the contained elements and grasps the distribution by irradiating the sample with an electron beam in a vacuum and measuring the characteristic X-rays generated. is there. EPMA can grasp how elements are distributed in a minute region, unlike grasping bulk (whole sample) elements as in chemical analysis (see, for example, Patent Document 1). ..
しかしながら、ＥＰＭＡを用いて試料における単体硫黄の分布を分析する場合、試料に真空中で電子線を照射することになるため、単体硫黄が昇華してしまうことがある。そのため、単体硫黄から発生する特性Ｘ線の強度が弱くなり、試料における単体硫黄の分布を精度よく分析することが困難となる。 However, when the distribution of elemental sulfur in a sample is analyzed using EPMA, the sample is irradiated with an electron beam in a vacuum, so that the elemental sulfur may sublimate. Therefore, the intensity of the characteristic X-rays generated from the elemental sulfur becomes weak, and it becomes difficult to accurately analyze the distribution of the elemental sulfur in the sample.
本発明は、昇華しやすい単体硫黄の分布を電子線の照射により分析する技術を提供することを目的とする。 An object of the present invention is to provide a technique for analyzing the distribution of elemental sulfur, which is easily sublimated, by irradiation with an electron beam.
本発明の第１の態様は、
試料に含まれる単体硫黄の分布を分析する単体硫黄分布の分析方法であって、
単体硫黄を含む試料に対し、照射電流量を２×１０−８Ａ以下として電子線を照射する照射工程と、
前記電子線の照射により前記試料から発生する特性Ｘ線を検出する検出工程と、
前記検出工程に基づいて、前記試料における前記単体硫黄の分布を分析する分析工程と、を有することを特徴とする、単体硫黄分布の分析方法が提供される。
The first aspect of the present invention is
It is an analysis method of elemental sulfur distribution that analyzes the distribution of elemental sulfur contained in a sample.
An irradiation step of irradiating a sample containing elemental sulfur with an electron beam with an irradiation current amount of 2 × 10-8 A or less,
A detection step of detecting characteristic X-rays generated from the sample by irradiation with the electron beam, and
Provided is a method for analyzing a simple substance sulfur distribution, which comprises an analysis step for analyzing the distribution of the elemental sulfur in the sample based on the detection step.
本発明の第２の態様は、第１の態様の単体硫黄分布の分析方法において、
前記照射工程および前記検出工程を電子線マイクロアナライザを用いて行う。
A second aspect of the present invention is the method for analyzing elemental sulfur distribution in the first aspect.
The irradiation step and the detection step are performed using an electron probe microanalyzer.
本発明の第３の態様は、第１又は第２の態様の単体硫黄分布の分析方法において、
前記試料が多孔質樹脂成形体である。
A third aspect of the present invention is the method for analyzing elemental sulfur distribution according to the first or second aspect.
The sample is a porous resin molded product.
本発明の第４の態様は、第１〜第３の態様のいずれか１つの単体硫黄分布の分析方法において、
前記照射工程では、前記電子線の照射電流量を２×１０−１０Ａ以上とする。
A fourth aspect of the present invention is the method for analyzing elemental sulfur distribution in any one of the first to third aspects.
In the irradiation step, the irradiation current amount of the electron beam is set to 2 × 10 -10 A or more.
本発明の第５の態様は、第１〜第４の態様のいずれか１つの単体硫黄分布の分析方法において、
前記照射工程では、前記電子線の照射電流量をａ［Ａ］、前記電子線を照射する照射時間をｂ［ｍｓｅｃ］としたとき、その積算値である照射量ａ×ｂが１×１０−６Ａ・ｍｓｅｃ以上１×１０−５Ａ・ｍｓｅｃ以下となるように前記電子線を照射する。
A fifth aspect of the present invention is the method for analyzing the elemental sulfur distribution in any one of the first to fourth aspects.
In the irradiation step, when the irradiation current amount of the electron beam is a [A] and the irradiation time for irradiating the electron beam is b [msec], the integrated value of the irradiation amount a × b is 1 × 10 −. 6 Irradiate the electron beam so as to be A · msec or more and 1 × 10 -5 A · msec or less.
本発明によれば、昇華しやすい単体硫黄の分布を電子線の照射により分析することができる。 According to the present invention, the distribution of elemental sulfur, which is easily sublimated, can be analyzed by irradiation with an electron beam.
例えば、工業製品の製造プロセスにおいて単体硫黄が残存する場合、環境への放出を防止する観点から製造プロセス中に単体硫黄がどの程度存在するのかを把握することが重要となる。 For example, when elemental sulfur remains in the manufacturing process of industrial products, it is important to understand how much elemental sulfur is present in the manufacturing process from the viewpoint of preventing release to the environment.
そこで、本発明者は、製造プロセスで採取した溶液を多孔質樹脂成形体（例えば、イオン交換樹脂膜など）に通過させ、このイオン交換樹脂膜に対して電子線を照射し、捕捉された単体硫黄から発生する特性Ｘ線を検出することにより、単体硫黄の分布を分析しようと試みた。 Therefore, the present inventor passes the solution collected in the manufacturing process through a porous resin molded body (for example, an ion exchange resin film), irradiates the ion exchange resin film with an electron beam, and captures the simple substance. An attempt was made to analyze the distribution of simple sulfur by detecting characteristic X-rays generated from sulfur.
しかし、上述したように、例えばＥＰＭＡにより、溶液を通過させたイオン交換樹脂膜（以下、試料という）に対して電子線を照射したところ、単体硫黄が昇華してしまうため、特性Ｘ線を十分に検出することができず、その分布を精度よく分析することができなかった。 However, as described above, when an ion exchange resin film (hereinafter referred to as a sample) through which a solution has passed is irradiated with an electron beam by, for example, EPMA, simple sulfur is sublimated, so that characteristic X-rays are sufficiently obtained. Could not be detected, and its distribution could not be analyzed accurately.
本発明者は、上記課題を解決すべく検討したところ、試料に電子線を照射するときの照射電流量を低くすることにより、試料に含まれる単体硫黄の昇華を抑制でき、その分布を分析できることを見出した。 As a result of studying to solve the above problems, the present inventor can suppress the sublimation of simple sulfur contained in the sample by lowering the irradiation current amount when irradiating the sample with an electron beam, and can analyze the distribution thereof. I found.
一般に、元素に電子線を照射して分析する場合、電子線の照射電流量が高いほど、電子線を照射したときに元素から発生する特性Ｘ線の強度が大きくなり、元素の検出感度がよくなる。例えば、鉱石中の金属の分布を分析する場合、照射電流量を２×１０−７Ａとする。しかし、本発明者の検討によると、単体硫黄では、照射電流量が２×１０−７Ａのように高いと昇華してしまうので、分析することが困難である。 In general, when an element is analyzed by irradiating it with an electron beam, the higher the irradiation current amount of the electron beam, the greater the intensity of the characteristic X-ray generated from the element when the element is irradiated, and the better the detection sensitivity of the element. .. For example, when analyzing the distribution of metals in ore, the irradiation current amount is 2 × 10-7 A. However, according to the study of the present inventor, it is difficult to analyze elemental sulfur because it sublimates when the irradiation current amount is as high as 2 × 10-7 A.
このことから、本発明者は照射電流量を適宜変更して検討したところ、照射電流量を２×１０−８Ａ以下とするとよいことを見出した。このような照射電流量で電子線を照射すると、ＥＰＭＡにて分析するのに問題とならない程度まで単体硫黄の昇華を抑制することができ、試料における単体硫黄の分布を分析することが可能となる。 From this, the present inventor found that the irradiation current amount should be 2 × 10-8 A or less as a result of examining by appropriately changing the irradiation current amount. When the electron beam is irradiated with such an irradiation current amount, the sublimation of elemental sulfur can be suppressed to the extent that it does not pose a problem for analysis by EPMA, and the distribution of elemental sulfur in the sample can be analyzed. ..
本発明は、上記知見に基づいて成されたものである。 The present invention has been made based on the above findings.
以下、本発明の一実施形態にかかる単体硫黄分布の分析方法について説明する。以下では、電子線マイクロアナライザ（ＥＰＭＡ）を用いて分析する場合について説明する。 Hereinafter, a method for analyzing the elemental sulfur distribution according to the embodiment of the present invention will be described. In the following, a case of analysis using an electron probe microanalyzer (EPMA) will be described.
本実施形態の分析方法において、評価対象となる試料は、単体硫黄を含むものであり、例えばイオン交換樹脂膜などの多孔質樹脂成形体であって、製造プロセスで採取された溶液を通過させ、単体硫黄が吸着したものである。 In the analysis method of the present embodiment, the sample to be evaluated contains elemental sulfur, for example, a porous resin molded body such as an ion exchange resin film, and is passed through a solution collected in the manufacturing process. Elemental sulfur is adsorbed.
本実施形態では、まず、試料として、単体硫黄を含む多孔質樹脂成形体を準備する。この試料にエポキシ系の樹脂（例えば、エポフィックス樹脂）を含浸させて固結させ、空孔に樹脂性分が充填された固結試料を得る。続いて、この固結試料の表面を研磨することにより、試料面を作製する。 In the present embodiment, first, a porous resin molded product containing elemental sulfur is prepared as a sample. This sample is impregnated with an epoxy resin (for example, epofix resin) and solidified to obtain a solidified sample in which the pores are filled with a resinous component. Subsequently, the surface of the consolidated sample is polished to prepare a sample surface.
続いて、ＥＰＭＡにて、固結試料の試料面に対して電子線を照射する。このとき、単体硫黄が昇華しないように、電子線の照射電流量を２×１０−８Ａ以下とする。このような照射電流量であれば、特性Ｘ線の検出に問題とならない程度まで単体硫黄の昇華を抑制することができる。 Subsequently, the sample surface of the consolidated sample is irradiated with an electron beam by EPMA. At this time, the amount of irradiation current of the electron beam is set to 2 × 10-8 A or less so that elemental sulfur does not sublimate. With such an irradiation current amount, sublimation of elemental sulfur can be suppressed to the extent that there is no problem in detecting characteristic X-rays.
照射電流量の下限値は特に限定されないが、２×１０−１０Ａ以上とすることが好ましい。このような照射電流量とすることにより、ノイズの影響を低減して鮮明な画像データを得ることができ、単体硫黄の分布をより精度良く分析することができる。 The lower limit of the irradiation current amount is not particularly limited, but is preferably 2 × 10 -10 A or more. By setting such an irradiation current amount, the influence of noise can be reduced and clear image data can be obtained, and the distribution of elemental sulfur can be analyzed more accurately.
また、本実施形態では、照射電流量を低くする分、試料に電子線を照射する照射時間を長くするとよい。一般に、照射電流量を低くすると、単体硫黄から発生する特性Ｘ線の強度が低くなり、得られる画像データが不鮮明となるおそれがあるが、照射時間を長くすることで、単体硫黄が受ける電子線の照射量を所定値以上として、鮮明な画像データを得ることができる。照射量とは、照射電流量をａ［Ａ］、照射時間をｂ［ｍｓｅｃ］としたとき、その積算値ａ×ｂを示す。鮮明な画像データを得る観点からは、照射量が１×１０−６Ａ・ｍｓｅｃ以上１×１０−５Ａ・ｍｓｅｃ以下となるように、照射電流量および照射時間を設定することが好ましい。このような照射量となるように電子線を照射することで、単体硫黄の昇華を抑制しつつ、単体硫黄からの特性Ｘ線の強度をノイズの影響を受けないレベルまで高めて鮮明な画像データを得ることができる。 Further, in the present embodiment, it is preferable to lengthen the irradiation time for irradiating the sample with the electron beam by the amount of lowering the irradiation current amount. Generally, when the amount of irradiation current is low, the intensity of characteristic X-rays generated from simple sulfur is low, and the obtained image data may be unclear. However, by lengthening the irradiation time, the electron beam received by single sulfur is received. Clear image data can be obtained by setting the irradiation amount of the above to a predetermined value or more. The irradiation amount indicates an integrated value a × b when the irradiation current amount is a [A] and the irradiation time is b [msec]. From the viewpoint of obtaining clear image data, it is preferable to set the irradiation current amount and the irradiation time so that the irradiation amount is 1 × 10 -6 A · msec or more and 1 × 10 -5 A · msec or less. By irradiating an electron beam with such an irradiation amount, the sublimation of elemental sulfur is suppressed, and the intensity of characteristic X-rays from elemental sulfur is increased to a level that is not affected by noise, resulting in clear image data. Can be obtained.
なお、照射時間としては、照射量が上記範囲となるように照射電流量に応じて適宜変更するとよく、例えば５０ｍｓｅｃ〜５００００ｍｓｅｃとするとよい。 The irradiation time may be appropriately changed according to the amount of irradiation current so that the irradiation amount falls within the above range, and may be, for example, 50 msec to 50,000 msec.
続いて、電子線の照射により、単体硫黄から発生する特性Ｘ線を検出する。本実施形態では、単体硫黄が昇華しないように電子線を照射しているので、検出するのに十分な強度を得ることができる。 Subsequently, characteristic X-rays generated from elemental sulfur are detected by irradiation with an electron beam. In the present embodiment, since the electron beam is irradiated so that the elemental sulfur does not sublimate, sufficient intensity for detection can be obtained.
続いて、検出した特性Ｘ線から、電子線を照射した試料面に分布する単体硫黄を分析する。本実施形態では、単体硫黄からの特性Ｘ線の強度が高いので、単体硫黄の分布を精度よく分析することができる。 Subsequently, the elemental sulfur distributed on the sample surface irradiated with the electron beam is analyzed from the detected characteristic X-rays. In the present embodiment, since the intensity of characteristic X-rays from elemental sulfur is high, the distribution of elemental sulfur can be analyzed with high accuracy.
本実施形態によれば、電子線の照射により昇華しやすい単体硫黄に、照射電流量を２×１０−８Ａ以下として電子線を照射している。これにより、単体硫黄からの特性Ｘ線の強度を高く維持しつつ、測定できるので、試料における単体硫黄の分布を精度よく分析することができる。 According to this embodiment, elemental sulfur, which is easily sublimated by irradiation with an electron beam, is irradiated with an electron beam with an irradiation current amount of 2 × 10-8 A or less. As a result, measurement can be performed while maintaining high intensity of characteristic X-rays from elemental sulfur, so that the distribution of elemental sulfur in the sample can be analyzed accurately.
以上、本発明の実施形態について説明してきたが、本発明は、上述した実施形態に何等限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々に改変することができる。 Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the gist of the present invention.
上記では、ＥＰＭＡを用いて分析する場合を例として説明したが、本発明は、これに限定されず、例えば、透過型電子顕微鏡（ＴＥＭ）やエネルギー分散型Ｘ線分光法（ＥＤＸ）などを用いて分析することも可能である。 In the above, the case of analysis using EPMA has been described as an example, but the present invention is not limited to this, and for example, a transmission electron microscope (TEM), an energy dispersive X-ray spectroscopy (EDX), or the like is used. It is also possible to analyze.
上記では、試料として単体硫黄を含む多孔質樹脂成形体を例として説明したが、本発明の分析対象はこれに限定されず、単体硫黄を含む試料であれば限定されない。 In the above, a porous resin molded product containing elemental sulfur has been described as an example, but the analysis target of the present invention is not limited to this, and the sample containing elemental sulfur is not limited.
以下、本発明をさらに詳細な実施例に基づき説明するが、本発明は、これら実施例に限定されない。 Hereinafter, the present invention will be described based on more detailed examples, but the present invention is not limited to these examples.
試料として、多孔質樹脂成形体内に単体硫黄が入り込んだものを準備した。この試料にエポフィックス冷間固結樹脂（丸本ストルアス株式会社製）を含浸させ、脱泡した後、１２時間硬化させることにより、固結試料を得た。その後、固結試料の表面を研磨することにより、電子線を照射する試料面を作製した。続いて、この試料面にカーボン蒸着を施し、ＥＰＭＡ（日本電子株式会社製造のＪＸＡ８１００）にて、試料面の面分析を行った。このときの測定条件としては、加速電圧を１５ｋＶ、照射電流量を２×１０−９Ａ、照射時間を２０００ｍｓｅｃ、照射量を４×１０−６Ａ・ｍｓｅｃ、測定元素をＳ（単体硫黄）とした。ＥＰＭＡによる面分析結果を図１に示す。図１は、ＥＰＭＡの面分析結果であり、本来赤色で示される硫黄の分布を黒で示したものである。 As a sample, a sample in which elemental sulfur had entered the porous resin molded body was prepared. This sample was impregnated with an Epofix cold-consolidating resin (manufactured by Marumoto Struas Co., Ltd.), defoamed, and then cured for 12 hours to obtain a consolidated sample. Then, the surface of the consolidated sample was polished to prepare a sample surface to be irradiated with an electron beam. Subsequently, carbon vapor deposition was performed on the sample surface, and the surface analysis of the sample surface was performed by EPMA (JXA8100 manufactured by JEOL Ltd.). The measurement conditions at this time were an accelerating voltage of 15 kV, an irradiation current amount of 2 × 10-9 A, an irradiation time of 2000 msec, an irradiation amount of 4 × 10-6 A · msec, and an element of measurement of S (elemental sulfur). did. The surface analysis result by EPMA is shown in FIG. FIG. 1 shows the results of surface analysis of EPMA, and the distribution of sulfur, which is originally shown in red, is shown in black.
比較例１では、ＥＰＭＡにて面分析を行う際に、照射量が実施例１と同じになるように照射電流量を２×１０−７Ａ、照射時間を２０ｍｓｅｃに変更した以外は、実施例１と同様に行った。つまり、比較例１では、実施例１と比べて照射電流量を大きく、かつ照射時間を短くしてＥＰＭＡによる面分析を行った。ＥＰＭＡによる面分析結果を図２に示す。 In Comparative Example 1, when performing surface analysis by EPMA, except that the amount of irradiation was changed in Example 1 the emission current amount to be the same as 2 × 10 -7 A, irradiation time 20 msec, Example The procedure was the same as in 1. That is, in Comparative Example 1, the surface analysis by EPMA was performed with a larger irradiation current amount and a shorter irradiation time as compared with Example 1. The results of surface analysis by EPMA are shown in FIG.
図１によれば、多孔質樹脂成形体に単体硫黄が分布している様子を確認することができた。
これに対して、図２では、硫黄の存在を示す黒部分がない。このことから、樹脂成形体内に分布している単体硫黄が、電子線の照射により昇華したものと思われる。
According to FIG. 1, it was possible to confirm that elemental sulfur was distributed in the porous resin molded body.
On the other hand, in FIG. 2, there is no black portion indicating the presence of sulfur. From this, it is considered that the elemental sulfur distributed in the resin molding body was sublimated by irradiation with an electron beam.
また、本発明者は、単体硫黄からなる試料片に対して、通常条件である、２×１０−７Ａの照射電流量で電子線を照射したところ、昇華により試料片が大きく縮むことが分かった。多孔質樹脂成形体に入り込んだ微細な単体硫黄は、比較例１のように通常条件の照射電流量で電子線を照射すると、昇華して消失しやすいものと考えられる。一方、実施例１のように照射電流量を小さくすれば、昇華したとしても縮みを抑制できるので、微細な単体硫黄を消失させることなく、分析できるものと考えられる。 Further, the present inventor found that when a sample piece made of elemental sulfur was irradiated with an electron beam under a normal condition of an irradiation current amount of 2 × 10 -7 A, the sample piece shrank significantly due to sublimation. It was. It is considered that the fine elemental sulfur that has entered the porous resin molded body is likely to sublimate and disappear when the electron beam is irradiated with the irradiation current amount under normal conditions as in Comparative Example 1. On the other hand, if the irradiation current amount is reduced as in Example 1, shrinkage can be suppressed even if sublimated, so it is considered that analysis can be performed without eliminating fine elemental sulfur.
このように、照射電流量を小さくすることにより、単体硫黄の昇華を、分析する際に問題とならない程度に抑制でき、試料に含まれる単体硫黄を精度よく分析できることが分かった。 As described above, it was found that by reducing the irradiation current amount, the sublimation of elemental sulfur can be suppressed to the extent that it does not cause a problem in the analysis, and the elemental sulfur contained in the sample can be analyzed accurately.
Claims (1)
単体硫黄を含む試料に対し、照射電流量を２×１０ −１０ Ａ以上２×１０−８Ａ以下として電子線を照射する照射工程と、
前記電子線の照射により前記試料から発生する特性Ｘ線を検出する検出工程と、
前記検出工程に基づいて、前記試料における前記単体硫黄の分布を分析する分析工程と、を有し、
前記単体硫黄を含む試料は、前記単体硫黄が吸着する多孔質樹脂成形体であり、
前記照射工程および前記検出工程では電子線マイクロアナライザを使用し、
前記照射工程では、前記電子線の照射電流量をａ［Ａ］、前記電子線を照射する照射時間をｂ［ｍｓｅｃ］としたとき、その積算値である照射量ａ×ｂが１×１０ −６ Ａ・ｍｓｅｃ以上１×１０ −５ Ａ・ｍｓｅｃ以下となるように前記電子線を照射する、単体硫黄分布の分析方法。 It is an analysis method of elemental sulfur distribution that analyzes the distribution of elemental sulfur contained in a sample.
An irradiation step of irradiating a sample containing elemental sulfur with an electron beam with an irradiation current amount of 2 × 10 -10 A or more and 2 × 10 -8 A or less.
A detection step of detecting characteristic X-rays generated from the sample by irradiation with the electron beam, and
On the basis of the detection process, have a, an analysis step of analyzing the distribution of the elemental sulfur in said sample,
The sample containing elemental sulfur is a porous resin molded product to which the elemental sulfur is adsorbed.
An electron probe microanalyzer was used in the irradiation step and the detection step.
In the irradiation step, when the irradiation current amount of the electron beam is a [A] and the irradiation time for irradiating the electron beam is b [msec], the integrated value of the irradiation amount a × b is 1 × 10 −. 6 A method for analyzing a single sulfur distribution, which irradiates the electron beam so as to be 1 × 10-5 A ・ msec or more and 1 × 10-5 A ・ msec or less .
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