この作品は、カナダ機器、発見とJMBNRBに授与Discovery Acceleratorの補助金は、カーネギー協会、ワシントンのポスドクフェローシップ·プログラムからの支援を認めるの自然科学工学研究評議会によってサポートされていました。スティーブンElardoも地球物理研究所のピストンシリンダープレスで撮影する前に、彼の支援を感謝しています。

著者は、開示することは何もありません。

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 border="0" cellpadding="0" cellspacing="0">
	<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>N/A</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>N/A</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>N/A</td>
			<td>Often sold as &#39;white glue&#39;</td>
		</tr>
		<tr>
			<td>Cyanoacrylate Glue</td>
			<td>e.g Krazy Glue/Loctite</td>
			<td>N/A</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 ZrO2 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&#160;</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 ...

metal-silicate-partitioning-at-high-pressure-temperature-experimental

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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

High-pressure Sapphire Cell for Phase Equilibria Measurements of CO2/Organic/Water Systems

The high pressure sapphire cell apparatus was constructed to visually determine the composition of multiphase systems without physical sampling. Specifically, the sapphire cell enables visual data collection from multiple loadings to solve a set of material balances to precisely determine phase composition. Ternary phase diagrams can then be established to determine the proportion of each component in each phase at a given condition. In principle, any ternary system can be studied although ternary systems (gas-liquid-liquid) are the specific examples discussed herein. For instance, the ternary THF-Water-CO2 system was studied at 25 and 40&#160;&#176;C and is described herein. Of key importance, this technique does not require sampling. Circumventing the possible disturbance of the system equilibrium upon sampling, inherent measurement errors, and technical difficulties of physically sampling under pressure is a significant benefit of this technique. Perhaps as important, the sapphire cell also enables the direct visual observation of the phase behavior. In fact, as the CO2 pressure is increased, the homogeneous THF-Water solution phase splits at about 2 MPa. With this technique, it was possible to easily and clearly observe the cloud point and determine the composition of the newly formed phases as a function of pressure.
The data acquired with the sapphire cell technique can be used for many applications. In our case, we measured swelling and composition for tunable solvents, like gas-expanded liquids, gas-expanded ionic liquids and Organic Aqueous Tunable Systems (OATS)1-4. For the latest system, OATS, the high-pressure sapphire cell enabled the study of (1) phase behavior as a function of pressure and temperature, (2) composition of each phase (gas-liquid-liquid) as a function of pressure and temperature and (3) catalyst partitioning in the two liquid phases as a function of pressure and composition. Finally, the sapphire cell is an especially effective tool to gather accurate and reproducible measurements in a timely fashion.

High-pressure Sapphire Cell for Phase Equilibria Measurements of CO2/Organic/Water Systems

The high pressure sapphire cell apparatus is a unique tool to study, without sampling, phase behavior under a wide range of pressures. Using a cathetometer, very precise volume measurements can be recorded to measure liquid expansion and phase composition. Thus, this synthetic method enables the study of (1) phase equilibria of multi-component mixtures and (2) the partition behavior of catalyst or model compounds as a function of pressure.

COの相平衡測定のための高圧サファイアセル<sub&gt; 2</sub&gt; /有機/水システム

The high pressure sapphire cell apparatus was constructed to visually determine the composition of multiphase systems without physical sampling. ...

化学

Ethylene Polymerizations Using Parallel Pressure Reactors and a Kinetic Analysis of Chain Transfer Polymerization

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel &#945;-diimine ethylene polymerization catalyst. Initial polymerizations with the catalyst lead to optimized reaction conditions, including catalyst concentration, ethylene pressure and reaction time. Using gas-uptake data for these reactions, a procedure to calculate the initial rate of propagation (kp) is presented. Using the optimized conditions, the ability of the nickel &#945;-diimine polymerization catalyst to undergo chain transfer with diethylzinc (ZnEt2) during ethylene polymerization was investigated. A procedure to assess the ability of the catalyst to undergo chain transfer (from molecular weight and 13C NMR data), calculate the degree of chain transfer, and calculate chain transfer rates (ke) is presented.

A protocol for the high-throughput analysis of polymerization catalyst, chain transfer polymerizations, polyethylene characterization, and reaction kinetic analysis is presented.

並列圧力反応器および連鎖移動重合の速度論的解析を使用してエチレン重合

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel ...

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

室温における炭素ナノシートの作製

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of trifluoromethoxylated aromatic compounds remains a formidable challenge in organic synthesis. Conventional approaches often suffer from poor substrate scope, or require use of highly toxic, difficult-to-handle, and/or thermally labile reagents. Herein, we report a user-friendly protocol for the synthesis of methyl 4-acetamido-3-(trifluoromethoxy)benzoate using 1-trifluoromethyl-1,2-benziodoxol-3(1H)-one (Togni reagent II). Treating methyl 4-(N-hydroxyacetamido)benzoate (1a) with Togni reagent II in the presence of a catalytic amount of cesium carbonate (Cs2CO3) in chloroform at RT afforded methyl 4-(N-(trifluoromethoxy)acetamido)benzoate (2a). This intermediate was then converted to the final product methyl 4-acetamido-3-(trifluoromethoxy)benzoate (3a) in nitromethane at 120 &#176;C. This procedure is general and can be applied to the synthesis of a broad spectrum of ortho-trifluoromethoxylated aniline derivatives, which could serve as useful synthetic building blocks for the discovery and development of new pharmaceuticals, agrochemicals, and functional materials.

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

An operationally simple procedure for the synthesis of ortho-trifluoromethoxylated aniline derivatives via a two-step sequence of O-trifluoromethylation of N-aryl-N-hydroxyacetamide followed by thermally induced intramolecular OCF3-migration is reported.

の合成のためのプロトコル<em&gt;オルソ</em&gt; -trifluoromethoxylatedアニリン誘導体

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

Rapid High-throughput Species Identification of Botanical Material Using Direct Analysis in Real Time High Resolution Mass Spectrometry

We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, and that these chemical fingerprints can be used for plant species identification. The mass spectral data can be acquired rapidly and in a high throughput manner without the need for sample extraction, derivatization or pH adjustment steps. The use of this technique bypasses challenges presented by more conventional techniques including lengthy chromatography analysis times and resource intensive methods. The high throughput capabilities of the direct analysis in real time-high resolution mass spectrometry protocol, coupled with multivariate statistical analysis processing of the data, provide not only class characterization of plants, but also yield species and varietal information. Here, the technique is demonstrated with two psychoactive plant products, Mitragyna speciosa (Kratom) and Datura (Jimsonweed), which were subjected to direct analysis in real time-high resolution mass spectrometry followed by statistical analysis processing of the mass spectral data. The application of these tools in tandem enabled the plant materials to be rapidly identified at the level of variety and species.

A method for species identification of botanical material by direct analysis in real time-high resolution mass spectrometry and multivariate statistical analysis is presented.

リアルタイム高分解能質量分析法で直接分析を用いた植物材料の急速なハイスループット種の同定

We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, ...

High Pressure Single Crystal Diffraction at PX^2

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB6. The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca0.51Na0.48)(Mg0.44Al0.44Fe2+0.14Fe3+0.02)Si2O6 sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 &#177;0.006 &#197;, b = 8.761 &#177;0.004 &#197;, c = 5.248 &#177;0.001 &#197;, &#946; = 105.06 &#177;0.03&#186;, &#945; = &#947; = 90&#186;.

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

PX ^ 2の高圧単結晶回折

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the ...

Non-equilibrium Microwave Plasma for Efficient High Temperature Chemistry

A flowing microwave plasma based methodology for converting electric energy into internal and/or translational modes of stable molecules with the purpose of efficiently driving non-equilibrium chemistry is discussed. The advantage of a flowing plasma reactor is that continuous chemical processes can be driven with the flexibility of startup times in the seconds timescale. The plasma approach is generically suitable for conversion/activation of stable molecules such as CO2, N2 and CH4. Here the reduction of CO2 to CO is used as a model system: the complementary diagnostics illustrate how a baseline thermodynamic equilibrium conversion can be exceeded by the intrinsic non-equilibrium from high vibrational excitation. Laser (Rayleigh) scattering is used to measure the reactor temperature and Fourier Transform Infrared Spectroscopy (FTIR) to characterize in situ internal (vibrational) excitation as well as the effluent composition to monitor conversion and selectivity.

This article describes a flowing microwave reactor that is used to drive efficient non-equilibrium chemistry for the application of conversion/activation of stable molecules such as CO2, N2 and CH4. The goal of the procedure described here is to measure the in situ gas temperature and gas conversion.

効率的な高温化学反応のための非平衡マイクロ波プラズマ

A flowing microwave plasma based methodology for converting electric energy into internal and/or translational modes of stable molecules with the purpose ...

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC)

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil quality, food flavoring, and human health. The biological activity of glucosinolates is released upon tissue damage, when they are mixed with the enzyme myrosinase. This results in the formation of pungent and toxic breakdown products, such as isothiocyanates and nitriles. Currently, more than 130 structurally different glucosinolates have been identified. The chemical structure of the glucosinolate is an important determinant of the product that is formed, which in turn determines its biological activity. The latter may range from detrimental (e.g., progoitrin) to beneficial (e.g., glucoraphanin). Each glucosinolate-containing plant species has its own specific glucosinolate profile. For this reason, it is important to correctly identify and reliably quantify the different glucosinolates present in brassicaceous leaf, seed, and root crops or, for ecological studies, in their wild relatives. Here, we present a well-validated, targeted, and robust method to analyze glucosinolate profiles in a wide range of plant species and plant organs. Intact glucosinolates are extracted from ground plant materials with a methanol-water mixture at high temperatures to disable myrosinase activity. Thereafter, the resulting extract is brought onto an ion-exchange column for purification. After sulfatase treatment, the desulfoglucosinolates are eluted with water and the eluate is freeze-dried. The residue is taken up in an exact volume of water, which is analyzed by high-pressure liquid chromatography (HPLC) with a photodiode array (PDA) or ultraviolet (UV) detector. Detection and quantification are achieved by conducting comparisons of the retention times and UV spectra of commercial reference standards. The concentrations are calculated based on a sinigrin reference curve and well-established response factors. The advantages and disadvantages of this straightforward method, when compared to faster and more technologically advanced methods, are discussed here.

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography HPLC

Here, we describe in great detail an established and robust protocol for the extraction of glucosinolates from ground plant materials. After an on-column sulfatase treatment of the extracts, the desulfoglucosinolates are eluted and analyzed by high-pressure liquid chromatography.

高圧液体クロマトグラフィー（HPLC）とグルコシノレートの抽出および分析のための簡単な方法

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil ...

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and related diseases, but their precise measurement is still a challenge. Many protocols have been described for neurotransmitter measurement by a variety of instruments, including high-pressure liquid chromatography (HPLC). However, there are shortcomings, such as complicated operation or hard-to-detect multiple targets, which cannot be avoided, and presently, the dominant analysis technique is still HPLC coupled with sensitive electrochemical or fluorimetric detection, due to its high sensitivity and good selectivity. Here, a detailed protocol is described for the pretreatment and detection of catecholamines with high pressure liquid chromatography with electrochemical detection (HPLC-ECD) in real urine samples of infants, using electrospun composite nanofibers composed of polymeric crown ether with polystyrene as adsorbent, also known as the packed-fiber solid phase extraction (PFSPE) method. We show how urine samples can be easily precleaned by a nanofiber-packed solid phase column, and how the analytes in the sample can be rapidly enriched, desorbed, and detected on an ECD system. PFSPE greatly simplifies the pretreatment procedures for biological samples, allowing for decreased time, expense, and reduction of the loss of targets. 
Overall, this work illustrates a simple and convenient protocol for solid-phase extraction coupled to an HPLC-ECD system for simultaneous determination of three monoamine neurotransmitters (norepinephrine (NE), epinephrine (E), dopamine (DA)) and two of their metabolites (3-methoxy-4-hydroxyphenylglycol (MHPG) and 3,4-dihydroxy-phenylacetic acid (DOPAC)) in infants' urine. The established protocol was applied to assess the differences of urinary catecholamines and their metabolites between high-risk infants with perinatal brain damage and healthy controls. Comparative analysis revealed a significant difference in urinary MHPG between the two groups, indicating that the catecholamine metabolites may be an important candidate marker for early diagnosis of cases at risk for brain damage in infants.

We present a convenient solid-phase extraction coupled to high-pressure liquid chromatography (HPLC) with electrochemical detection (ECD) for simultaneous determination of three monoamine neurotransmitters and two of their metabolites in infants' urine. We also identify the metabolite MHPG as a potential biomarker for the early diagnosis of brain damage for infants.

抽出と神経伝達物質カテコールアミン及びその代謝物の高速液体クロマトグラフィーによる分析のための便利な方法

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and ...

Experimental Methods for Efficient Solar Hydrogen Production in Microgravity Environment

Long-term space flights and cis-lunar research platforms require a sustainable and light life-support hardware which can be reliably employed outside the Earth's atmosphere. So-called 'solar fuel' devices, currently developed for terrestrial applications in the quest for realizing a sustainable energy economy on Earth, provide promising alternative systems to existing air-revitalization units employed on the International Space Station (ISS) through photoelectrochemical water-splitting and hydrogen production. One obstacle for water (photo-) electrolysis in reduced gravity environments is the absence of buoyancy and the consequential, hindered gas bubble release from the electrode surface. This causes the formation of gas bubble froth layers in proximity to the electrode surface, leading to an increase in ohmic resistance and cell-efficiency loss due to reduced mass transfer of substrates and products to and from the electrode. Recently, we have demonstrated efficient solar hydrogen production in microgravity environment, using an integrated semiconductor-electrocatalyst system with p-type indium phosphide as the light-absorber and a rhodium electrocatalyst. By nanostructuring the electrocatalyst using shadow nanosphere lithography and thereby creating catalytic 'hot spots' on the photoelectrode surface, we could overcome gas bubble coalescence and mass transfer limitations and demonstrated efficient hydrogen production at high current densities in reduced gravitation. Here, the experimental details are described for the preparations of these nanostructured devices and further on, the procedure for their testing in microgravity environment, realized at the Bremen Drop Tower during 9.3 s of free fall.

Efficient solar-hydrogen production has recently been realized on functionalized semiconductor-electrocatalyst systems in a photoelectrochemical half-cell in microgravity environment at the Bremen Drop Tower. Here, we report the experimental procedures for manufacturing the semiconductor-electrocatalyst device, details of the experimental set-up in the drop capsule and the experimental sequence during free fall.

微小重力環境における効率的な太陽水素製造のための実験方法

Long-term space flights and cis-lunar research platforms require a sustainable and light life-support hardware which can be reliably employed outside the ...