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ここで概説したプロトコルを使用して実行包含無実験の結果は、以前の文献29（OS、イリジウム、金）、30（RE、Au）と31（PT）における文献データと比較しました。 Ptが封入フリーラン製品の有用性を実証する中で最も有益です。低Fの O 2で動作する実験では、Ertel ら 48は、安定した原点に介在物が割り当てられ、したがって、時間分解LA-IC...

地上降着は、月の形成の1,2の責任と思っ巨大なインパクトの段階で終了、コンドライトバルク組成と微惑星同士の衝突のシリーズとして発生したと考えられています。衝撃によるプロト地球の加熱と短命の同位体の崩壊は、大規模な溶融を引き起こすのに十分であったとFeに富む金属溶融物を密これを通してマグマオーシャンや池の形成が下る可能性があります。マグマオーシャンのベースに到達すると、金属溶融物はレオロジー境界、ストールが発生し、最終的に成長しているコア2の固体マントルを通って下降する前に、最後の金属ケイ酸塩平衡を受けます。金属溶融物のような金属とケイ酸塩相の間のさらなる化学通信は、マントルの固体部分が大きいため大きさや金属ダイアピル3の急激な下降に排除されると考えられて横断します。金属コアとケイMANTに地球のこの一次微分6 -ルは、地球物理学および地球化学観測4の両方で、今日明らかにされています。マグマオーシャンのベースの金属ケイ酸塩均衡のためのもっともらしい条件を得るために、これらの観​​察の解釈は、しかし、実験結果の適切なデータベースを必要とします。 プリミティブ上部マントル（PUM）は、コア形成のケイ酸残基を含む仮想的なリザーバーであり、その組成物は、したがって、金属ケイ酸塩平衡中の微量元素の挙動を反映しています。微量元素は、それらの地球化学的親和性に基づいて、コアの分離の際に金属とケイ酸塩溶融物との間に分布しています。金属相のための要素の嗜好の大きさは、金属ケイ酸塩の分配係数によって記述することができます<img alt="式（1）" src="/files/ftp_upload/52725/52725eq1.jpg" /><img alt="式（2）" src="/files/ftp_upload/52725/52725eq2.jpg" /> （1） どこ<img alt="式3" src="/files/ftp_upload/52725/52725eq3.jpg" />と<img alt="式4" src="/files/ftp_upload/52725/52725eq4.jpg" /> 私は金属とケイ酸塩でそれぞれ溶融元素の濃度を示します。の値<img alt="式（5）" src="/files/ftp_upload/52725/52725eq5.jpg" /> &gt; 1は、親鉄（鉄を愛する）の動作と、それらの&lt;1親石（岩を愛する）の挙動を示しています。要素を親鉄PUM組成ショーの推定値は、典型的には、地球のバルク組成6,8の代表として考えコンドライト7、に関連して枯渇しています。この枯渇は、コアによって親鉄元素の隔離によるもので、耐熱性元素のためにその大きさは、直接の値を反映する必要があります<img alt="式（5）" src="/files/ftp_upload/52725/52725eq5.jpg" /> 。研究室の実験は、従って値を決定しよう<img alt="式（5）" src="/files/ftp_upload/52725/52725eq5.jpg" /> RAの上圧力（P）、温度（T）と酸素フガシティー（Fの O 2）マグマの海の底からの金属の分離に関連する条件のNGE。 T - -これらの実験の結果は、Pの領域を描写するために使用することができるO 2空間fは複数の親鉄元素（ 例えば 、9から11）のPUMの豊富と互換性があること。 マグマオーシャンのシナリオに関連する高い圧力および温度は、ピストン·シリンダまたはマルチアンビルプレスのいずれかを使用して実験室で再現することができます。ピストン·シリンダ装置は、適度な圧力（〜2万気圧）と高温（〜2573 K）条件へのアクセスを提供しますが、大量の試料と容易に使用するカプセルの様々な材料を可能にします。急冷速度も、このように実行の製品のテクスチャーの解釈を簡素化、ガラスのケイ酸塩メルト組成物の範囲のクエンチングを可能にします。マルチアンビル装置は、典型的には、より小さなサンプル·ボリュームを採用したが、適切なアセンブリの設計で〜27 GPaでと〜3,000 Kの温度、これらのメソッドの使用があることを適度にやや親鉄元素の多くに分割データを許可しているまでの圧力を達成することができますT条件 - Pの広い範囲にわたって集まりました。これらのデータに基づいて、PUM組成の予測は正確な値に依存したモデルであるが、金属ケイ酸塩平衡は、それぞれ〜29 GPaで3000 Kを超える平均圧力および温度条件で発生を示唆しています。特定の酸化還元に敏感な要素のPUM存在量を考慮するためには（ 例えば、V、Crの）は、F、O 2はまた、共存する鉄とウスタイト（のFeOによって課されている以下〜4から2対数単位から降着中に進化すると考えられています）同等のPT条件 （鉄ウスタイトバッファ）で12。 MのPUMの豊富さが、いずれかの親鉄元素が深いマグマオーシャンの基部に金属ケイ酸塩の平衡によって説明することができる、それがこのような状況でも最も高度に親鉄元素（のHSE）に適用されるかどうかを評価することは困難であることが判明しました。低圧（P〜0.1 MPa）とし、温度（T &lt;1,673 K）の実験で示した鉄金属のためのHSEの極端な親和性は、ケイ酸塩の地球が強く、これらの要素に枯渇する必要があるということです。 PUM用HSE内容の推定値は、しかし、（ 図1）コンドライトへの唯一の中等度の枯渇を相対的に示しています。見かけHSE過剰に一般的に仮定解決策は、地球は、コア形成13以降のコンドライト物質の後期降着を経験したことがあります。この後期増額材料はPUMと混合し、HSEの濃度が上昇したが、より豊富な要素にほとんど影響を持っていただろう。あるいは、それは非常に親鉄のHSEの性質が低いPで示すことが示唆されています</em&gt; - Tの実験は、核形成14,15の間に存在する高PT条件に保持されません。これらの仮説をテストするために、実験を適切な条件でのHSEの溶解性および金属ケイ酸塩のパーティションを決定するために行われなければなりません。しかし、多くの以前の研究で急冷ラン製品の珪酸塩部分の汚染、ラン製品の分析を複雑にし、金属とケイ酸塩溶融物との間のHSEのための真の分配係数を不明瞭にしています。 のHSEが自然に適切な濃度レベルで存在しているパーティションの実験では、鉄金属のためのこれらの要素の極端な嗜好は、ケイ酸塩溶融物中で、その測定値を防ぐことができます。この問題を回避するために、溶解度の測定は、ケイ酸塩溶融物は、目的とする値のHSEに飽和している作られ<img alt="式（5）" src="/files/ftp_upload/52725/52725eq5.jpg" />ボリソフらの形式主義を使用して計算されますアル。16。ケイ酸塩が還元条件で行わHSEの溶解度実験から、製品を実行急冷し、しかし、多くの場合、分散されたHSE±Feは17を介在物による汚染の証拠が表示されます。低Fの Oでこれらの介在物のPt、Irの、OS、ReおよびRuを、（ 例えば 、18から27）を含む2つの実験の近くに偏在にもかかわらず、それらのテクスチャープレゼンテーションの研究間の顕著なばらつきがあります。例22および26を参照するために比較します。それは介在物は、実験28の運転条件で安定相である生成することができることが実証されているが、試料を急冷されると、これは、封入体の形成を排除するものではありません。介在物の起源を取り巻く不確実性は、分析結果の治療を困難にし、減少珪酸塩が溶けでのHSEの真の溶解度にわたって曖昧さにつながっています。インクルージョンフリーラン製品は、評価するために必要とされますその研究は、正確な溶解HSE濃度をもたらす分析的アプローチを採用しています。 31 -還元条件下で金属介在物の生成を抑制することにはかなりの進歩は、現在のサンプル設計は出発物質29にAuやSiのいずれかを添加することによって、以前の研究から修正されたピストン·シリンダ装置を用いた実験で証明されています。出発材料にAuや単体Siを添加すると、それぞれの実験のサンプルの幾何学的形状または f の O 2発生を変化させます。これらの方法には、拡散試料還元対HSEのタイミングを変更することによって、金属介在物の生成を抑制することを目的としており、ベネットら 31で説明されています。このような機械的に支援平衡と遠心分離ピストン·シリンダとして介在物の珪酸塩メルトを浄化するためにいくつかの以前の試みとは異なり、本プロトコルは、特殊明朝することなく実施することができますatusとは、 高温高圧実験に適しています。 ここでは詳細に説明は、高温（&gt; 1,873 K）、2万気圧とのものと同様のF O 2のシリケート溶融物中のRe、Osの、イリジウム、ルテニウム、白金および金の溶解度を決定するためのピストンシリンダーベースのアプローチであります鉄ウスタイトバッファ。同様の実験計画の適用はまた、必要な位相関係を提供する湿潤特性を、他の圧力でHSE実験に成功したことを証明することができ、運動の関係は、選択された条件に存続します。既存のデータは、しかし、私たちのサンプルデザインは、深いマグマオーシャンに対応する圧力で成功するかどうかを予測するには不十分です。また概説は適度に、わずかに親鉄元素（MSE及びSSEそれぞれ）、マルチアンビル装置を使用してパーティションを決定するために使用される一般的なアプローチです。高圧へのHSE用封入フリーセットの拡張は、同様のマルチアンビル方法を採用する可能性があります。水着エーテル、これらの手順は、コア - 分離の条件と地上降着の段階の両方を制限する手段を提供します。

<table><tbody><tr><td>G10 Epoxy/Fiberglass Sheet</td><td>Accurate plastics, Inc.</td><td>GEES.020N.3648</td><td></td></tr><tr><td>Powdered starting materials- -Oxides, metals, carbonates</td><td>Alfa Aesar</td><td>Specific to desired experiment</td><td></td></tr><tr><td>Castable 2-part MgO ceramic</td><td>Aremco</td><td>Ceramcast - 584</td><td></td></tr><tr><td>PTFE Dry Lubricant</td><td>Camie-Campbell</td><td>2000 TFE-Coat</td><td></td></tr><tr><td>Graphite resistance heaters</td><td>Carbone of America (Now owned by Mersen USA)</td><td>Custom Order</td><td></td></tr><tr><td>Barium Carbonate</td><td>Chemical Products Corporation</td><td>Custom Order</td><td>Calcined free-flowing (CFF) grade</td></tr><tr><td>C-Type Thermocouple Wire (W26%Re, W5%Re)</td><td>Concept Alloys</td><td></td><td>~0.25 mm diameter is suitable for most experiments</td></tr><tr><td>Zirconia Cement</td><td>Cotronics; Resbond 940 2-part cement</td><td></td><td>Use 100 parts powder for every 25 to 28 parts activator</td></tr><tr><td>Polyvinyl Acetate (PVA) Glue</td><td>e.g., Bostik</td><td></td><td>Often sold as &#039;white glue&#039;</td></tr><tr><td>Cyanoacrylate Glue</td><td>e.g., Krazy Glue/Loctite</td><td></td><td></td></tr><tr><td>Piston cylinder pressure vessel and WC piston</td><td>Hi-Quality Carbide Tooling Inc.</td><td>Custom Order</td><td></td></tr><tr><td>Silica Glass Tubing</td><td>Quartz Plus</td><td>Custom Order</td><td></td></tr><tr><td>Crushable ZrO&lt;sub&gt;2&lt;/sub&gt; tubes</td><td>Saint-Gobain</td><td>Custom Order</td><td></td></tr><tr><td>Crushable MgO rods and tubes</td><td>Saint-Gobain</td><td>Custom Order</td><td></td></tr><tr><td>WC cubes for multi-anvil experiments</td><td>Tungaloy</td><td>Custom Order</td><td>Cubes are grade-F WC alloy</td></tr><tr><td>Single hole alumina tube for multi-anvil thermocouple</td><td>Vesuvius McDanel</td><td>AXS071730-04-06</td><td></td></tr><tr><td>4-hole alumina tube for piston cylinder thermocouple</td><td>Vesuvius McDanel</td><td>AXF1159--07-12&amp;nbsp;</td><td></td></tr><tr><td>4-hole alumina tube for multi-anvil thermocouple</td><td>Vesuvius McDanel</td><td>AXF1159-04-06</td><td></td></tr></tbody></table>

metal-silicate partitioning at high pressure and temperature: experimental methods and a protocol to suppress highly siderophile element inclusions

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from their extraction to the core during terrestrial accretion. Experiments to investigate the partitioning of these elements between metal and silicate melts suggest that the PUM composition is best matched if metal-silicate equilibrium occurred at high pressures and temperatures, in a deep magma ocean environment. The behavior of the most highly siderophile elements (HSEs) during this process however, has remained enigmatic. Silicate run-products from HSE solubility experiments are commonly contaminated by dispersed metal inclusions that hinder the measurement of element concentrations in the melt. The resulting uncertainty over the true solubility and metal-silicate partitioning of these elements has made it difficult to predict their expected depletion in PUM. Recently, several studies have employed changes to the experimental design used for high pressure and temperature solubility experiments in order to suppress the formation of metal inclusions. The addition of Au (Re, Os, Ir, Ru experiments) or elemental Si (Pt experiments) to the sample acts to alter either the geometry or rate of sample reduction respectively, in order to avoid transient metal oversaturation of the silicate melt. This contribution outlines procedures for using the piston-cylinder and multi-anvil apparatus to conduct solubility and metal-silicate partitioning experiments respectively. A protocol is also described for the synthesis of uncontaminated run-products from HSE solubility experiments in which the oxygen fugacity is similar to that during terrestrial core-formation. Time-resolved LA-ICP-MS spectra are presented as evidence for the absence of metal-inclusions in run-products from earlier studies, and also confirm that the technique may be extended to investigate Ru. Examples are also given of how these data may be applied.

ケイ酸塩でHSEの溶解度を決定するために以下の実施例および実験の議論の焦点は、低Fの O 2で溶融します。 T - -芯金分離の2条件O fを 、読者は参考文献9を参照され-図11 図7B-Dバック表示、マルチアンビル実験からMSE及びSSE分割データPを拘束するために使用することができる方法の総合的な例について典型的な実験ランの?...

Watch this Scientific Journal Video about Metal-silicate Partitioning at High Pressure and Temperature: Experimental Methods and a Protocol to Suppress Highly Siderophile Element Inclusions at JoVE.co

Metal-silicate Partitioning at High Pressure and Temperature: Experimental Methods and a Protocol to Suppress Highly Siderophile Element Inclusions

We present a procedure to determine the metal-silicate partitioning of siderophile elements, emphasizing techniques that suppress the formation of metal inclusions in experiments for the noble metals. The results of these experiments are used to demonstrate the effect of core-formation on the highly siderophile element composition of the mantle.

高温高圧下における金属珪酸塩パーティション化：実験方法と非常に親鉄元素介在物を抑制するためのプロトコル

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from ...

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12.4K ビュー.  University of Toronto. We present a procedure to determine the metal-silicate partitioning of siderophile elements, emphasizing techniques that suppress the formation of metal inclusions in experiments for the noble metals. The results of these experiments are used to demonstrate the effect of core-formation on the highly siderophile element composition of the mantle.

ビデオ: Metal-silicate Partitioning at High Pressure and Temperature: Experimental Methods and a Protocol to Suppress Highly Siderophile Element Inclusions

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

エクストリーム圧力と温度での合成とMicrodiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

工学

Simulation of the Planetary Interior Differentiation Processes in the Laboratory

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process.

The high-pressure and high-temperature experiments described here mimic planet interior differentiation processes. The processes are visualized and better understood by high-resolution 3D imaging and quantitative chemical analysis.

研究室での惑星インテリア分化過程のシミュレーション

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to ...

Experimental Column Setup for Studying Anaerobic Biogeochemical Interactions Between Iron (Oxy)Hydroxides, Trace Elements, and Bacteria

Fate and speciation of trace elements (TEs), such as arsenic (As) and mercury (Hg), in aquifers are closely related to physio-chemical conditions, such as redox potential (Eh) and pH, but also to microbial activities that can play a direct or indirect role on speciation and/or mobility. Indeed, some bacteria can directly oxidize As(III) to As(V) or reduce As(V) to As(III). Likewise, bacteria are strongly involved in Hg cycling, either through its methylation, forming the neurotoxin monomethyl mercury, or through its reduction to elemental Hg&#176;. The fates of both As and Hg are also strongly linked to soil or aquifer composition; indeed, As and Hg can bind to organic compounds or (oxy)hydroxides, which will influence their mobility. In turn, bacterial activities such as iron (oxy)hydroxide reduction or organic matter mineralization can indirectly influence As and Hg sequestration. The presence of sulfate/sulfide can also strongly impact these particular elements through the formation of complexes such as thio-arsenates with As or metacinnabar with Hg.
Consequently, many important questions have been raised on the fate and speciation of As and Hg in the environment and how to limit their toxicity. However, due to their reactivity towards aquifer components, it is difficult to clearly dissociate the biogeochemical processes that occur and their different impacts on the fate of these TE.
To do so, we developed an original, experimental, column setup that mimics an aquifer with As- or Hg-iron-oxide rich areas versus iron depleted areas, enabling a better understanding of TE biogeochemistry in anoxic conditions. The following protocol gives step by step instructions for the column set-up either for As or Hg, as well as an example with As under iron and sulfate reducing conditions.

Experimental Column Setup for Studying Anaerobic Biogeochemical Interactions Between Iron OxyHydroxides, Trace Elements, and Bacteria

Fate and speciation of arsenic and mercury in aquifers are closely related to physio-chemical conditions and microbial activity. Here, we present an original experimental column setup that mimics an aquifer and enables a better understanding of trace element biogeochemistry in anoxic conditions. Two examples are presented, combining geochemical and microbiological approaches.

(オキシ) 鉄の水酸化物、微量元素、細菌の嫌気性生物地球化学的相互作用を研究するため実験的列の設定

Fate and speciation of trace elements (TEs), such as arsenic (As) and mercury (Hg), in aquifers are closely related to physio-chemical conditions, such as ...

環境学

High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature (&#62; 300 &#176;C). However, because of the low stress resolution of current solid-pressure-medium apparatuses, high-resolution measurements are today restricted to low-pressure deformation experiments in the gas-pressure-medium apparatus. A new generation of solid-medium piston-cylinder (&#34;Griggs-type&#34;) apparatus is here described. Able to perform high-pressure deformation experiments up to 5 GPa and designed to adapt an internal load cell, such a new apparatus offers the potential to establish a technological basis for high-pressure rheology. This paper provides video-based detailed documentation of the procedure (using the &#34;conventional&#34; solid-salt assembly) to perform high-pressure, high-temperature experiments with the newly designed Griggs-type apparatus. A representative result of a Carrara marble sample deformed at 700 &#176;C, 1.5 GPa and 10-5 s-1 with the new press is also given. The related stress-time curve illustrates all steps of a Griggs-type experiment, from increasing pressure and temperature to sample quenching when deformation is stopped. Together with future developments, the critical steps and limitations of the Griggs apparatus are then discussed.

Rock deformation needs to be quantified at high pressure. A description of the procedure to perform deformation experiments in a newly designed solid-medium Griggs-type apparatus is here given. This provides technological basis for future rheological studies at pressures up to 5 GPa.

新世代グリッグス型装置を使用して、高温高圧変形実験

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature ...

Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation

An approach for acquiring more reliable X-ray photoelectron spectroscopy data from corrosion inhibitor/metal interfaces is described. More specifically, the focus is on metallic substrates immersed in acidic solutions containing organic corrosion inhibitors, as these systems can be particularly sensitive to oxidation following removal from solution. To minimize the likelihood of such degradation, samples are removed from solution within a glove box purged with inert gas, either N2 or Ar. The glove box is directly attached to the load-lock of the ultra-high vacuum X-ray photoelectron spectroscopy instrument, avoiding any exposure to the ambient laboratory atmosphere, and thus reducing the possibility of post immersion substrate oxidation. On this basis, one can be more certain that the X-ray photoelectron spectroscopy features observed are likely to be representative of the in situ submerged scenario, e.g. the oxidation state of the metal is not modified.

A protocol to avoid the oxidation of metallic substrates during sample transfer from an inhibited acidic solution to an X-ray photoelectron spectrometer is presented.

XPSで腐食防止剤/金属界面の化学組成を決定する：最小化後のイマージョン酸化

An approach for acquiring more reliable X-ray photoelectron spectroscopy data from corrosion inhibitor/metal interfaces is described. More specifically, ...

化学

An Experimental Protocol for Studying Mineral Effects on Organic Hydrothermal Transformations

Organic-mineral interactions are widely occurring in hydrothermal environments, such as hot springs, geysers on land, and the hydrothermal vents in the deep ocean. Roles of minerals are critical in many hydrothermal organic geochemical processes. Traditional hydrothermal methodology, which includes using reactors made of gold, titanium, platinum, or stainless-steel, is usually associated with the high cost or undesired metal catalytic effects. Recently, there is a growing tendency for using the cost-effective and inert quartz or fused silica glass tubes in hydrothermal experiments. Here, we provide a protocol for carrying out organic-mineral hydrothermal experiments in silica tubes, and we describe the essential steps in the sample preparation, experimental setup, products separation, and quantitative analysis. We also demonstrate an experiment using a model organic compound, nitrobenzene, to show the effect of an iron-containing mineral, magnetite, on its degradation under a specific hydrothermal condition. This technique can be applied to study complex organic-mineral hydrothermal interactions in a relatively simple laboratory system.

Earth-abundant minerals play important roles in the natural hydrothermal systems. Here, we describe a reliable and cost-effective method for the experimental investigation of organic-mineral interactions under hydrothermal conditions.

有機水熱変換のミネラル効果を研究するための実験プロトコル

Organic-mineral interactions are widely occurring in hydrothermal environments, such as hot springs, geysers on land, and the hydrothermal vents in the ...

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

高炉スラグの双方向の物価安定政策：沈殿した炭酸カルシウムおよびゼオライト重金属吸着剤の合成

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

Atom Probe Tomography Analysis of Exsolved Mineral Phases

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in lamellae exsolved from host mineral phases. Thus, the analysis of the orientation, size, morphology, composition and spacing of exsolution lamellae is an area of active research in the geosciences. The conventional study of these lamellae has been conducted by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and more recently with focused ion beam (FIB)-based nanotomography, yet with limited chemical information. Here, we explore the use of atom probe tomography (APT) for the nanoscale analysis of ilmenite exsolution lamellae in igneous titanomagnetite from ash deposits erupted from the active Soufri&#232;re Hills Volcano (Montserrat, British West Indies). APT allows the precise calculation of interlamellar spacings (14&#8211;29 &#177; 2 nm) and reveals smooth diffusion profiles with no sharp phase boundaries during the exchange of Fe and Ti/O between the exsolved lamellae and the host crystal. Our results suggest that this novel approach permits nanoscale measurements of lamellae composition and interlamellar spacing that may provide a means to estimate the lava dome temperatures necessary to model extrusion rates and lava dome failure, both of which play a key role in volcanic hazard mitigation efforts.

Analysis of the morphology, composition, and spacing of exsolution lamellae can provide essential information to understand geological processes related to volcanism and metamorphism. We present a novel application of APT for the characterization of such lamellae and compare this approach to the conventional use of electron microscopy and FIB-based nanotomography.

エクスブソリュート鉱物相の原子プローブ断層撮影解析

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in ...

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

Ex その場その場で調査構造変換の方法: 金属ガラスの結晶化の事例

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

表面有機金属化学の方法論を用いてシリカ支持触媒によるイミンメタセシス

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...