JP6477166B2 - Mineral composition evaluation method - Google Patents
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本発明は、鉱物の組成評価方法に関し、特に熱分解する鉱物の組成の変化を、ＸＡＦＳ測定により評価する、鉱物の組成評価方法である。 The present invention relates to a mineral composition evaluation method, and more particularly to a mineral composition evaluation method in which a change in the composition of a thermally decomposable mineral is evaluated by XAFS measurement.
鉱物の組成を評価する方法には、Ｘ線回折（ＸＲＤ）を用いて鉱物の結晶構造を解析することが一般的に行われている。また、Ｘ線を利用した他の分析方法としても、蛍光Ｘ線元素分析法（ＸＲＦ）により、鉱物に含まれている元素を分析する方法が行われている。 As a method for evaluating the composition of a mineral, it is a common practice to analyze the crystal structure of the mineral using X-ray diffraction (XRD). As another analysis method using X-rays, a method of analyzing elements contained in minerals by fluorescent X-ray elemental analysis (XRF) has been performed.
Ｘ線回折では、粉末Ｘ線回折の回折パターンを、最小二乗法を用いてフィッティングするなど、所謂、リートベルト解析を用いることで、構造解析や各相の定量測定などが可能である。 In X-ray diffraction, structural analysis, quantitative measurement of each phase, and the like are possible by using a so-called Rietveld analysis such as fitting a diffraction pattern of powder X-ray diffraction using a least square method.
一方、鉱物の一種であるドロマイトは、焼成したドロマイトと未焼成のものとを比較した場合、焼成した方が各種重金属等に対し優れた吸着能を示すことが知られている。また、特開２０１２−１５７８３４号公報（特許文献１）には、半焼成ドロマイトを用いた６価セレンや６価クロムなどの重金属イオンの除去剤が開示されている。 On the other hand, dolomite, which is a kind of mineral, is known to exhibit superior adsorption ability for various heavy metals when calcined dolomite is compared with unfired dolomite. JP 2012-157834 A (Patent Document 1) discloses a removal agent for heavy metal ions such as hexavalent selenium and hexavalent chromium using semi-baked dolomite.
また、ドロマイトは、次の２つの式に示すように二段階で熱分解することが知られている。
ＣａＭｇ（ＣＯ３）２→ＣａＣＯ３＋ＭｇＯ＋ＣＯ２ ・・・（１）
ＣａＣＯ３＋ＭｇＯ＋ＣＯ２→ＣａＯ＋ＭｇＯ＋２ＣＯ２ ・・・（２）
In addition, dolomite is known to thermally decompose in two stages as shown in the following two equations.
CaMg (CO 3 ) 2 → CaCO 3 + MgO + CO 2 (1)
CaCO 3 + MgO + CO 2 → CaO + MgO + 2CO 2 (2)
例えば、ドロマイトの重金属等の吸着性能を調べるには、熱分解の進行状況に応じて、逐次、鉱物の組成を評価する方法が必要となる。しかも、ドロマイトの熱分解は、一度に全体が進行するのではなく局所的に進行すること、しかも、上述のように２段階の熱分解が進行していることから、特に、定常的な結晶構造を分析するＸＲＤでは、ドロマイトの焼成状態を組成評価する手法としては、不十分である。 For example, in order to examine the adsorption performance of dolomite such as heavy metals, a method for sequentially evaluating the composition of minerals is required according to the progress of thermal decomposition. In addition, the thermal decomposition of dolomite proceeds locally rather than at once, and since the two-stage thermal decomposition proceeds as described above, in particular, a steady crystal structure. XRD is not sufficient as a method for evaluating the composition of the firing state of dolomite.
本発明の目的は、上記課題を解決し、熱分解により組成が変化する、ドロマイトのような鉱物の組成を、全体の鉱物組成の変化ではなく、局所的な構造変化、例えば表層やバルク等においても評価して、ＸＲＤと並列して用いて、鉱物の組成の変化が詳細に解析することができる、新規な鉱物の組成評価方法を提供することである。 The object of the present invention is to solve the above-mentioned problems, and to change the composition of a mineral such as dolomite, which changes in composition by thermal decomposition, in a local structural change, such as a surface layer or a bulk, not a change in the overall mineral composition It is also intended to provide a novel mineral composition evaluation method that can be used in parallel with XRD to analyze changes in mineral composition in detail.
本発明者らは、鋭意研究を行った結果、熱分解する鉱物をＸＡＦＳ測定、特にＸＡＮＥＳ測定を利用することで、鉱物の局所的構造解析を行うことができ、ＸＲＤ方法と並列で用いることで、より正確な鉱物の組成変化が評価できることを見出したものである。 As a result of diligent research, the present inventors have been able to perform local structural analysis of minerals by utilizing XAFS measurement, particularly XANES measurement, for minerals that are thermally decomposed. It has been found that a more accurate change in composition of minerals can be evaluated.
即ち、本発明の鉱物の組成評価方法は、以下に示す技術的特徴を有している。
（１） 熱分解により組成が変化する鉱物の組成を評価する方法であって、該鉱物を加熱しながら、第１の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第１のＸＡＦＳスペクトルパターンを取得し、前記第１の特定時間と異なる第２の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第２のＸＡＦＳスペクトルパターンを取得し、第１のＸＡＦＳスペクトルパターンと第２のＸＡＦＳスペクトルパターンとを比較して、該鉱物に含まれる特定の化合物に関し、該鉱物における局所構造の組成を評価することを特徴とする、鉱物の組成評価方法である。
That is, the mineral composition evaluation method of the present invention has the following technical features.
(1) A method for evaluating the composition of a mineral whose composition changes due to thermal decomposition, wherein the mineral is irradiated with X-rays measured by XAFS measurement while sweeping the wavelength at a first specific time while heating the mineral. The first XAFS spectral pattern is acquired, and the second XAFS spectral pattern is irradiated at a second specific time different from the first specific time while irradiating the mineral while sweeping the wavelength of X-rays by XAFS measurement. And comparing the first XAFS spectral pattern with the second XAFS spectral pattern to evaluate the composition of the local structure in the mineral with respect to a specific compound contained in the mineral, It is a composition evaluation method.
（２） 上記（１）に記載の鉱物の組成評価方法において、熱により組成が変化する鉱物は、炭酸塩鉱物又は層状粘土鉱物であることを特徴とする。 (2) The mineral composition evaluation method according to (1) above, wherein the mineral whose composition is changed by heat is a carbonate mineral or a layered clay mineral.
（３） 上記（１）又は（２）に記載の鉱物の組成評価方法において、該鉱物はドロマイトであり、該鉱物に含まれる特定の化合物はＭｇＯであり、ＸＡＦＳスペクトルパターンはマグネシウムのＫ吸収端ＸＡＮＥＳスペクトルを用いて、ドロマイトの組成を評価することを特徴とする。 (3) In the mineral composition evaluation method according to the above (1) or (2), the mineral is dolomite, the specific compound contained in the mineral is MgO, and the XAFS spectrum pattern is a magnesium K absorption edge. The composition of dolomite is evaluated using XANES spectrum.
（４） 上記（１）の鉱物の組成評価方法は、ＸＡＦＳスペクトルパターンは、全電子収量測定法と蛍光収量測定法を備え、該全電子収量測定法により該鉱物の表面の組成を、該蛍光収量測定法により該鉱物のバルクの組成を各々評価することを特徴とする。 (4) The mineral composition evaluation method described in ( 1 ) above is such that the XAFS spectral pattern includes a total electron yield measurement method and a fluorescence yield measurement method, and the mineral surface composition is determined by the total electron yield measurement method. The bulk composition of the mineral is evaluated by a yield measurement method.
本発明は、熱分解により組成が変化する鉱物の組成を評価する方法であって、該鉱物を特定温度で連続的に加熱しながら、第１の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第１のＸＡＦＳスペクトルパターンを取得し、前記第１の特定時間と異なる第２の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第２のＸＡＦＳスペクトルパターンを取得し、第１のＸＡＦＳスペクトルパターンと第２のＸＡＦＳスペクトルパターンとを比較することで、該鉱物に含まれる特定の化合物に関し、該鉱物における局所構造の組成を評価することが可能となる。特に、ＸＡＦＳスペクトルパターンを利用することで、鉱物の局所的な構造変化を詳細に解析できるため、異なる時間の複数のＸＡＦＳスペクトルパターンを比較することで、鉱物の組成変化を詳細に解析することが可能となる。 The present invention relates to a method for evaluating the composition of a mineral whose composition changes due to thermal decomposition, in which X-rays obtained by XAFS measurement are wavelength-swept at a first specific time while the mineral is continuously heated at a specific temperature. While irradiating the mineral, a first XAFS spectrum pattern is obtained, and the mineral is irradiated while sweeping the wavelength of X-rays by XAFS measurement at a second specific time different from the first specific time. The second XAFS spectral pattern is obtained, and the composition of the local structure in the mineral is evaluated with respect to a specific compound contained in the mineral by comparing the first XAFS spectral pattern with the second XAFS spectral pattern. It becomes possible to do. In particular, since the local structural change of mineral can be analyzed in detail by using the XAFS spectral pattern, the composition change of mineral can be analyzed in detail by comparing a plurality of XAFS spectral patterns at different times. It becomes possible.
以下、本発明の鉱物の組成評価方法について、好適例を用いて詳細に説明する。
本発明の鉱物の組成評価方法は、熱分解により組成が変化する鉱物の組成を評価する方法であって、該鉱物を加熱しながら、第１の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第１のＸＡＦＳスペクトルパターンを取得し、前記第１の特定時間と異なる第２の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第２のＸＡＦＳスペクトルパターンを取得し、第１のＸＡＦＳスペクトルパターンと第２のＸＡＦＳスペクトルパターンとを比較して、該鉱物に含まれる特定の化合物に関し、該鉱物における局所構造の組成を評価することを特徴とする。
Hereinafter, the mineral composition evaluation method of the present invention will be described in detail using preferred examples.
The mineral composition evaluation method of the present invention is a method for evaluating the composition of a mineral whose composition changes due to thermal decomposition, and sweeps X-rays by XAFS measurement at a first specific time while heating the mineral. While irradiating the mineral, a first XAFS spectrum pattern is obtained, and the mineral is irradiated while sweeping the wavelength of X-rays by XAFS measurement at a second specific time different from the first specific time. Obtaining a second XAFS spectral pattern and comparing the first XAFS spectral pattern with the second XAFS spectral pattern to evaluate the composition of the local structure in the mineral for a specific compound contained in the mineral It is characterized by that.
鉱物を加熱する方法については、特に限定はされないが、継続的に変化を観察する場合には、特定の温度で連続的に熱を鉱物に加える方法が採用できる。当然、所定の温度で熱を加えた後で測定し、再度、同じ温度又は異なる温度で熱を加えた後に測定するなど、断続的に熱を加える方法もある。本発明では、ＸＡＦＳ測定を採用しているため、鉱物を粉末に加工するなど処理工程は不要であるため、鉱物の熱分解による組成変化をどのような温度環境で測定するかという、測定目的に応じて種々の加熱方法が採用できる。 The method for heating the mineral is not particularly limited, but when continuously observing the change, a method in which heat is continuously applied to the mineral at a specific temperature can be employed. Of course, there is also a method of applying heat intermittently, such as measuring after applying heat at a predetermined temperature and then measuring again after applying heat at the same or different temperature. In the present invention, since XAFS measurement is adopted, a processing step such as processing of a mineral into a powder is not required. Therefore, for the measurement purpose of measuring in what temperature environment the composition change due to thermal decomposition of the mineral is measured. Various heating methods can be adopted accordingly.
ＸＡＦＳ測定とは、Ｘ線吸収微細構造（X-ray absorption fine structure）測定方法を意味し、Ｘ線吸収端近傍構造（Ｘ線スペクトルで、吸収端から短波長側の約３０ｅＶ程度に亘る領域に見られる微細構造。ＸＡＮＥＳ）と、Ｘ線吸収広域微細構造（Ｘ線スペクトルで、吸収端の短波長側の約３０ｅＶ程度から１ｋｅＶに亘る領域に見られる減衰する波状の振動構造。ＥＸＡＦＳ）とがある。本発明では、特に、ＸＡＮＥＳスペクトルを用いることが好ましい。 XAFS measurement means a measurement method of X-ray absorption fine structure (X-ray absorption fine structure), in the vicinity of the X-ray absorption edge (in the X-ray spectrum, about 30 eV from the absorption edge to the short wavelength side). XANES) and X-ray absorption broad-area microstructure (X-ray spectrum, damped wave-like vibrational structure, EXAFS) seen in the region from about 30 eV to 1 keV on the short wavelength side of the absorption edge. is there. In the present invention, it is particularly preferable to use the XANES spectrum.
また、ＸＡＦＳ測定に係る測定法は、試料電流による全電子収量法（ＴＥＹ）と蛍光収量法（ＰＦＹ）がある。全電子収量測定法は、鉱物の表面の組成を測定するのに適しており、蛍光収量測定法は、鉱物のバルクの組成を測定するのに適している。 In addition, the measurement methods related to the XAFS measurement include a total electron yield method (TEY) by a sample current and a fluorescence yield method (PFY). The total electron yield measurement method is suitable for measuring the composition of the surface of the mineral, and the fluorescence yield measurement method is suitable for measuring the bulk composition of the mineral.
本発明の鉱物の組成評価方法は、熱により組成が変化する鉱物の構造解析又は組成評価に用いることが好ましい。具体的には、炭酸塩鉱物や層状粘土鉱物などが挙げられ、以下の実施例でも示すように、ドロマイトの組成評価には特に有効である。 The mineral composition evaluation method of the present invention is preferably used for structural analysis or composition evaluation of a mineral whose composition changes due to heat. Specific examples include carbonate minerals and layered clay minerals, which are particularly effective for evaluating the composition of dolomite, as shown in the following examples.
本発明の鉱物の組成評価方法は、次に示す手順（１）〜（３）で実施する。
（１）鉱物を加熱しながら、第１の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第１のＸＡＦＳスペクトルパターンを取得する。
（２）第１の特定時間と異なる第２の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第２のＸＡＦＳスペクトルパターンを取得する。
（３）第１のＸＡＦＳスペクトルパターンと第２のＸＡＦＳスペクトルパターンとを比較して、鉱物に含まれる特定の化合物に関し、鉱物における局所構造の組成を評価する。
The mineral composition evaluation method of the present invention is carried out by the following procedures (1) to (3).
(1) While heating the mineral, the first XAFS spectrum pattern is obtained by irradiating the mineral while sweeping the wavelength of X-rays measured by XAFS at the first specific time.
(2) The second XAFS spectrum pattern is obtained by irradiating the mineral while sweeping the wavelength of X-rays by XAFS measurement at a second specific time different from the first specific time.
(3) The first XAFS spectral pattern and the second XAFS spectral pattern are compared, and the composition of the local structure in the mineral is evaluated for a specific compound contained in the mineral.
具体的に説明すると、例えば、加熱する前（未焼成状態。特定時間としては、焼成開始からの経過時間が０分に相当。）に、Ｘ線を吸収端付近のエネルギーレベルから短波長側に数十ｅＶのエネルギー範囲で、波長掃引しながら鉱物に照射する。鉱物からの全電子収量又は蛍光収量を測定し、ＸＡＦＳスペクトルパターンを取得する。 More specifically, for example, before heating (unbaked state. As the specific time, the elapsed time from the start of firing is equivalent to 0 minutes), X-rays are moved from the energy level near the absorption edge to the short wavelength side. The mineral is irradiated in the energy range of several tens of eV while sweeping the wavelength. The total electron yield or fluorescence yield from the mineral is measured, and the XAFS spectral pattern is obtained.
次に、鉱物を所定の温度で加熱しながら、例えば、所定時間（例えば、数分〜数十分）の間隔で、定期的に、上述したＸ線の照射と同じ方法で照射し、ＸＡＦＳスペクトルパターンを取得する。そして、集まった複数のＸＡＦＳスペクトルパターンを分析する。具体的には、スペクトルピーク値の移動（ピークを示すＸ線エネルギーレベルの変化。熱分解で発生する特定分子に対応するエネルギーレベルでのスペクトルパターンの変化）を検出（観察）したり、着目している特定分子のＸＡＦＳスペクトルパターンと測定したＸＡＦＳスペクトルパターンの一致性を評価し、特定分子の存在を確認する。 Next, while heating the mineral at a predetermined temperature, for example, at a predetermined time (for example, several minutes to several tens of minutes) at regular intervals, the mineral is irradiated in the same manner as the X-ray irradiation described above, and the XAFS spectrum Get the pattern. Then, a plurality of collected XAFS spectral patterns are analyzed. Specifically, it detects (observes) the movement of the spectrum peak value (change in the X-ray energy level indicating the peak. Change in the spectrum pattern at the energy level corresponding to the specific molecule generated by thermal decomposition) The coincidence between the XAFS spectral pattern of the specific molecule and the measured XAFS spectral pattern is evaluated, and the presence of the specific molecule is confirmed.
本発明の鉱物の組成評価方法を用いて、実際に、ドロマイトの組成分析を行った。以下に、具体的な実験方法を紹介する。
（試料作成）
電気炉を用い、大気中、温度１０７３Ｋにおいて焼成時間を５〜３００分の間で変化させドロマイトを焼成した。
The composition analysis of dolomite was actually performed using the mineral composition evaluation method of the present invention. The specific experimental method is introduced below.
(Sample preparation)
Using an electric furnace, the dolomite was fired in the atmosphere at a temperature of 1073 K with the firing time varied between 5 and 300 minutes.
（Ｘ線回折のリートベルト法による分析）
得られた各種焼成試料をＸ線回折（PANalytical X' Pert Pro MPD）に供し、リートベルト解析により各相の定量を行った。その結果を表１に示す。
(X-ray diffraction analysis by Rietveld method)
The various fired samples obtained were subjected to X-ray diffraction (PANalytical X 'Pert Pro MPD), and each phase was quantified by Rietveld analysis. The results are shown in Table 1.
（実験）
ドロマイトの構成成分であるＣａ及びＭｇのＫ吸収端ＸＡＦＳをそれぞれ、立命館大学ＳＲセンターＢＬ−３及びＢＬ−１０を用いて測定した。分光結晶は、ＣａのＫ吸収端測定においてＳｉ（１１１）を用い、ＭｇのＫ吸収端測定においてＢｅｒｙｌ（１０−１０）及びＫＴＰ（０１１）を用いた。
測定法は、全電子収量（ＴＥＹ）及び蛍光収量（ＰＦＹ）にて行った。
(Experiment)
The K absorption edges XAFS of Ca and Mg, which are dolomite constituents, were measured using Ritsumeikan University SR Center BL-3 and BL-10, respectively. The spectroscopic crystal used Si (111) in the measurement of the K absorption edge of Ca, and Beryl (10-10) and KTP (011) in the measurement of the K absorption edge of Mg.
The measurement method was performed by total electron yield (TEY) and fluorescence yield (PFY).
（実験結果及び考察）
表１のリートベルト解析の結果から、焼成３０〜４０分の間に、ドロマイトの上述した熱分解反応（１）は完了したと判断される。別途、ＴＧ−ＤＳＣ分析を行ったところ、この判断を裏付けるデータも得られた。
(Experimental results and discussion)
From the results of the Rietveld analysis in Table 1, it is determined that the above-described thermal decomposition reaction (1) of dolomite has been completed within 30 to 40 minutes of firing. Separately, when TG-DSC analysis was performed, data supporting this judgment was also obtained.
図１に、各種焼成試料のＭｇのＫ吸収端ＸＡＮＥＳのスペクトルパターンを示す。バルクの情報を多く含むＰＦＹ測定では、焼成５分までは未焼成ドロマイト（ｒａｗ）と類似したスペクトル（１３１３ｅＶ付近にピークを持つ）を示す。２０分焼成試料では、ＭｇＯに類似した１３０９ｅＶ付近のピークが出現する。焼成時間が３０分より長い焼成試料では、２０分焼成試料よりも顕著に１３０９ｅＶ付近のピークが観測される。また、スペクトルパターンは、焼成が進むに従い、試薬ＭｇＯのスペクトルパターンに近くなり、ＭｇＯがバルク中に多く存在していると判断される。 In FIG. 1, the spectrum pattern of Mg K absorption edge XANES of various baking samples is shown. The PFY measurement including a large amount of bulk information shows a spectrum (having a peak in the vicinity of 1313 eV) similar to that of unfired dolomite (raw) until 5 minutes of firing. In the sample fired for 20 minutes, a peak around 1309 eV similar to MgO appears. In the fired sample with a firing time longer than 30 minutes, a peak near 1309 eV is observed more markedly than in the 20-minute fired sample. Further, the spectrum pattern becomes closer to the spectrum pattern of the reagent MgO as the calcination proceeds, and it is determined that a large amount of MgO is present in the bulk.
図２に示す、表面敏感であるＴＥＹ測定では、５分焼成試料で既にＭｇＯに類似した１３０９ｅＶ付近のシャープなピークが出現している。このことから、５分までにドロマイトの表面では、局所構造変化が始まっていると判断される。 In the surface sensitive TEY measurement shown in FIG. 2, a sharp peak in the vicinity of 1309 eV, which is similar to MgO, has already appeared in the sample fired for 5 minutes. From this, it is determined that the local structural change has started on the surface of dolomite by 5 minutes.
図３に、各種焼成試料のＣａのＫ吸収端ＸＡＮＥＳ（ＰＦＹ）のスペクトルパターンを示す。未焼成ドロマイトと、５，３０，６０分焼成試料のスペクトルパターンは、ほぼ同様である。よって、焼成前後におけるＣａ原子周りの局所構造は、平均としては、ほとんど変化していないと考えられる。この結果から上述したドロマイトの熱分解反応（２）に示すＣａＯの生成は、少なくとも焼成６０分より後に起こると考えられる。この考察は、表１のリートベルト解析結果と一致している。 In FIG. 3, the spectrum pattern of K K absorption edge XANES (PFY) of various baking samples is shown. The spectral patterns of the unfired dolomite and the fired sample for 5, 30, 60 minutes are almost the same. Therefore, the local structure around the Ca atoms before and after firing is considered to have hardly changed on average. From this result, it is considered that the generation of CaO shown in the above-described thermal decomposition reaction (2) of dolomite occurs at least after 60 minutes of calcination. This consideration is consistent with the Rietveld analysis results in Table 1.
これらの結果から、焼成前後でＣａ原子周りの局所構造には、ほとんど変化が見られなかったが、Ｍｇ原子周りの局所構造は焼成時間の経過に伴って変化することが分かった。さらに、ＰＦＹ測定とＴＥＹ測定では、ＭｇのＫ吸収端ＸＡＮＥＳのスペクトルパターンが、異なる変化を示すことが判明した。よって、ドロマイトを焼成することにより生成したＭｇＯは、最表面とバルクとでは、異なる構造を有していることが判断された。 From these results, it was found that there was almost no change in the local structure around the Ca atom before and after firing, but the local structure around the Mg atom changed with the lapse of the firing time. Further, it was found that the spectrum pattern of the Mg K absorption edge XANES shows different changes in the PFY measurement and the TEY measurement. Therefore, it was judged that MgO produced | generated by baking a dolomite has a different structure in an outermost surface and a bulk.
以上の実験結果からも、ドロマイトの焼成に伴う局所的な構造解析について、ＸＡＦＳ測定方法を用いた本発明の鉱物の組成評価方法が有効に機能していることが分かった。 Also from the above experimental results, it was found that the mineral composition evaluation method of the present invention using the XAFS measurement method functions effectively for local structural analysis accompanying calcination of dolomite.
以上説明したように、本発明によれば、熱分解により組成が変化する、ドロマイトのような鉱物の組成を、全体の鉱物組成の変化ではなく、局所的な構造変化、例えば表層やバルク等においても評価して、ＸＲＤと並列して用いて、鉱物の組成の変化が詳細に解析することができる、新規な鉱物の組成評価方法を提供することができる。 As described above, according to the present invention, the composition of a mineral such as dolomite whose composition changes due to thermal decomposition is not a change in the overall mineral composition, but a local structural change such as a surface layer or a bulk. It is also possible to provide a novel mineral composition evaluation method that can be used in parallel with XRD to analyze in detail the change in mineral composition.
Claims (3)
該鉱物を加熱しながら、
第１の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第１のＸＡＦＳスペクトルパターンを取得し、
前記第１の特定時間と異なる第２の特定時間において、ＸＡＦＳ測定によるＸ線を波長掃引しながら該鉱物に照射して、第２のＸＡＦＳスペクトルパターンを取得し、
第１のＸＡＦＳスペクトルパターンと第２のＸＡＦＳスペクトルパターンとを比較して、該鉱物に含まれる特定の化合物に関し、該鉱物における局所構造の組成を評価する方法であって、
該ＸＡＦＳスペクトルパターンは、全電子収量測定法と蛍光収量測定法を備え、該全電子収量測定法により該鉱物の表面の組成を、該蛍光収量測定法により該鉱物のバルクの組成を各々評価することを特徴とする、鉱物の組成評価方法。 A method for evaluating the composition of a mineral whose composition changes due to thermal decomposition,
While heating the mineral,
At a first specific time, the mineral is irradiated with X-rays measured by XAFS while wavelength sweeping to obtain a first XAFS spectral pattern;
In a second specific time different from the first specific time, the mineral is irradiated with X-rays by XAFS measurement while wavelength sweeping to obtain a second XAFS spectral pattern,
A method of comparing a first XAFS spectral pattern with a second XAFS spectral pattern to evaluate the composition of the local structure in the mineral for a specific compound contained in the mineral ,
The XAFS spectral pattern includes a total electron yield measurement method and a fluorescence yield measurement method, and the mineral surface composition is evaluated by the total electron yield measurement method, and the bulk composition of the mineral is evaluated by the fluorescence yield measurement method. A method for evaluating the composition of minerals.
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