이 작품은 JMBNRB에게 수여 자연 과학 및 캐나다 장비, 검색 및 디스커버리 액셀러레이터 보조금 공학 연구위원회에 의해 지원되었다 워싱턴 포스트 박사 교제 프로그램의 카네기 연구소의 지원을 인정합니다. 스티븐 Elardo 또한 지구 물리학 연구소에서 피스톤 실린더 프레스로 촬영하기 전에 자신의 도움에 감사합니다.

저자가 공개하는 게 없다.

여기에 설명 된 프로토콜을 사용하여 수행 포함없는 실험의 결과는 이전의 참조도 29의 (O를 · IR), 금 (Au), (30) (재), 금 (Au) 및 (31) (PT)의 문헌 데이터와 비교되었다. 백금은 포함이없는 실행 제품의 유용성을 입증에 가장 유익하다. 로우 F의 O 2 실행 실험을 위해, Ertel 외. (48)는 안정적으로 원점 개재물을 할당하므로 시분 LA-ICPMS 스펙트럼 최저 ?...

지상파 증가는 달의 형성 1, 2에 대한 책임을 생각 거대한 충격 단계에서 종료, chondritic 벌크 조성 행성 체 사이의 충돌의 시리즈로 발생한 것으로 생각된다. 충격에 의한 원시 지구와 수명이 짧은 동위 원소의 붕괴 난방 광범위한 용융 마그마 바다와 철 풍부한 금속의 용융이 내려 수 조밀 통해 연못의 형성을 야기하기에 충분했다. 마그마 바다의 바닥에 도달하면, 금속 용융은 유동 학적 경계, 실속 발생, 결국 성장 코어 2 고체 맨틀을 통해 내려 전에 최종 금속 규산염 평형을받을. 용융 금속과 같은 금속 실리케이트 상간 또한 화학 통신 맨틀의 중실 부 인해 대형 금속 다이아 퍼 (3)의 급속한 하강에 배제되는 것으로 생각된다 횡단. 금속 코어 및 규산염 녀 mant에 지구의이 차 분화6 - 제작은 모두 지구 물리학 및 지구 화학적 관찰 (4)에 의해 오늘 공개된다. 마그마 바다의 바닥에 금속 규산염 평형에 대한 설득력있는 조건을 산출하기 위해 이러한 관찰을 해석하지만, 실험 결과의 적절한 데이터베이스가 필요합니다. 프리미티브 상부 맨틀 (PUM)는 코어 형성 실리케이트 잔기를 갖는 가상의 저장이며 따라서 그 조성은 금속 규산염 평형 중에 미량 원소의 동작을 반영한다. 미량 원소는 그 화학적 친화도에 근거하여 코어 편 중에 용융 금속 규산염 사이에 분포된다. 금속 상에 대한 기본 요소의 크기는 금속 실리케이트 분배 계수에 의해 설명 될 수 있습니다 <img alt="식 (1)" src="/files/ftp_upload/52725/52725eq1.jpg" /><img alt="식 (2)" src="/files/ftp_upload/52725/52725eq2.jpg" /> (1) 어디에 <img alt="식 (3)" src="/files/ftp_upload/52725/52725eq3.jpg" /> 과 <img alt="식 (4)" src="/files/ftp_upload/52725/52725eq4.jpg" /> 나는 금속 규산염 각각 녹아 원소의 농도를 나타낸다. 의 값 <img alt="식 (5)" src="/files/ftp_upload/52725/52725eq5.jpg" /> &gt; 1 siderophile (철 사랑)의 행동과 그 &lt;1 lithophile (바위 사랑) 동작을 나타냅니다. 요소를 siderophile PUM 조성 쇼의 추정은 일반적으로 지구의 대량 구성 6,8의 대표로 간주 구립 운석 7에 상대적으로 고갈된다. 이 고갈 핵심으로 siderophile 요소의 격리로 인해, 내화물 요소의 크기는 직접 값을 반영해야 <img alt="식 (5)" src="/files/ftp_upload/52725/52725eq5.jpg" /> . 실험실 실험은 따라서의 값을 결정하고자 <img alt="식 (5)" src="/files/ftp_upload/52725/52725eq5.jpg" /> RA 이상압력 (P), 온도 (T)와 산소 분압 (f를 O 2) 마그마 바다의 기지에서 금속 분리와 관련된 조건의 NGE. T - -이 실험의 결과는 다음의 P 영역을 서술하기 위해 사용될 수있다 F의 O를 여러 siderophile 소자 PUM 풍부와 호환이 공간 (예를 들어, 9-11). 높은 압력과 마그마 바다 시나리오에 관련된 온도는 피스톤 실린더 또는 다중 모루 프레스를 사용하여 실험실에서 재현 할 수 있습니다. 피스톤 실린더 장치는 중간 압 (~ 2 GPA) 및 고온 (2573 ~ K)의 조건에 대한 액세스를 제공하지만, 대규모 샘플 볼륨과 용이하게 사용될 수있는 캡슐 재료의 다양성을 가능하게한다. 빠른 냉각 속도는 따라서 런 제품의 조직 해석을 단순화로 실리케이트 유리 조성물의 용융 범위의 소광을 허용한다.멀티 모루 장치는 일반적으로 작은 샘플 볼륨을 사용하지만 적절한 어셈블리 설계와 압력에 ~ 27 GPa의와 ~ 3,000 케이의 온도 이러한 방법의 사용은 적당히의 많은 파티션의 데이터를 허용하고 약간 요소가 될 siderophile있다을 달성 할 수있다 T 조건 - (P)의 넓은 범위에 걸쳐 모였다. 이들 데이터에 기초 PUM 조성물의 예측 모델이 정확한 값 의존하더라도 금속 규산염 평형 각각 ~ 초과 평균 압력 및 온도 조건에서 29 GPa 인 3000 K를 발생 시사한다. (예를 들면, V, CR) 2는 또한 공존 철, 위스 타이트에 의해 부과 된 그 아래 ~ 4-2 로그 단위에서 증가하는 동안 진화를 생각하는 f를 O (특정 산화 환원에 민감한 요소의 PUM의 풍요 로움에 대한 FeO의를 설명하기 위해 ) 상당 PT 조건 (철 위스 타이트 버퍼) 12. 비록 M의 PUM 풍부어떤 siderophile 요소가 깊은 마그마 바다의 바닥에 금속 규산염 평형에 의해 설명 될 수 있습니다, 그것은이 상황이 또한 가장 높은 siderophile 요소 (HSES)에 적용하는 경우 평가하기 어려운 입증했다. 낮은 압력 (P ~ 0.1 MPa의) 및 온도 (T &lt;1673 K) 실험에 의해 표시 철 금속 HSES의 극단적 인 친 화성 규산 지구가 강하게 이러한 요소 고갈해야합니다 제안합니다. PUM위한 HSE 콘텐츠의 추정은, 그러나, (도 1) 콘드 라이트 만 적당한 공핍 대하여 나타낸다. 명백한 HSE 초과에 일반적으로 상정 솔루션은 지구가 핵심 형성 (13) 이후 chondritic 재료의 늦은 증가를 경험한다는 것이다. 이 늦은 인한이자 재료는 PUM와 혼합 HSE 농도를 상승하지만, 더 풍부한 요소에 무시할 영향을했을 것이다. 또는, HSES의 매우 낮은 자연 siderophile P로 나타낸 것이 제안되었다 </em&gt; - T 실험 코어 형성 14, 15 중에 존재하는 높은 PT 상태로 유지되지 않습니다. 이러한 가설을 검증하기 위하여, 실험은 적절한 조건에서 HSES의 용해도 및 금속 실리케이트 분할을 결정하기 위해 수행되어야한다. 그러나 많은 선행 연구에서 담금질 실행 제품의 규산염 부분의 오염, 실행 제품 분석을 복잡하고 금속과 규산염 용융물 사이 HSES에 대한 진정한 분배 계수를 가려있다. HSES 자연에 적합한 농도 수준에 존재하는 파티션 실험에서, 철 금속에 대한 이러한 요소의 극단적 인 기본 설정은 규산염 용융 자신의 측정을 방지 할 수 있습니다. 이 문제를 회피하기 위해, 용해도 측정은 관심의 값 HSE에있는 규산염 용융물이 포화 만들어진다 <img alt="식 (5)" src="/files/ftp_upload/52725/52725eq5.jpg" /> 보리 소프의 등의 형식주의를 사용하여 계산등. (16). 환원 조건에서 수행 HSE 용해도 실험으로부터 담금질 실리케이트 런 제품, 그러나 종종 분산 HSE ± 철에 의한 오염에 대한 근거를 표시하는 17 개재물. 낮은 F 오에서 이러한 개재물의 가까운 편재에도 불구하고 태평양 표준시의 Ir, O를, 다시와의 Ru를 포함하는이 실험은, (예를 들어, 18-27), 자신의 조직 프레젠테이션의 연구 사이에 주목할만한 변화가있다; 예를 들어 22, 26 참조를 비교합니다. 이 개재물은 실험 28의 실행 조건에서 안정한 상을 형성 할 수있는 것으로 입증되었지만, 샘플 켄칭 될 때,이 개재물의 형성을 배제하는 것은 아니다. 개재물의 원점 주변 불확실성 분석 결과의 처리가 곤란하게하고, 감소 된 실리케이트 녹에 HSES의 진정한 용해도 이상 모호하게되었다. 포함이없는 실행 제품은 평가해야합니다어떤 연구는 정확한 용해 HSE 농도를 산출 분석 접근 방식을 채택하고있다. 31 - 환원 조건에서 금속 개재물의 형성을 억제하는데 상당한 진전 이제 샘플 디자인이 원료 (29)의 Au 또는 Si를 추가하여 기존의 연구에서 개정하는 피스톤 - 실린더 장치를 이용한 실험에서 입증되었다. 출발 물질에 금이나 원소의 Si 첨가는 각각의 실험 샘플 기하학 또는 F O 2 진화를 바꾼다. 이들 방법은 샘플에 확산 환원 대 HSE의 타이밍을 변경하여 금속 개재물 형성을 억제하도록 구성되며, 베넷 외. (31)에서 논의된다. 이러한 기계적으로 지원 평형 및 원심 분리 피스톤 실린더와 같은 내포물의 규산염 용융물을 정화하는 몇 가지 이전의 시도와는 달리, 본 프로토콜은 전문 appar없이 구현 될 수있다ATUS과 높은 PT 실험에 적합합니다. 여기에 상세히 기재된 고온 (&gt; 1873 K), 2 GPa의과 유사한 F의 O 2에서 규산염 용융물에 재현하여 OS,의 Ir, Ru로, Pt 및 Au로의 용해도를 결정하기 위해 피스톤 - 실린더 기반 접근법 철 위스 타이트 버퍼. 유사한 실험 설계의 응용 프로그램은 또한, 요구되는 위상 관계를 제공하는 특성을 습윤제, 다른 압력에서 HSE 실험에서 성공적인 증명할 수 있고 운동 관계는 선택 조건으로 유지. 그러나 기존 데이터는, 우리의 샘플 디자인은 깊은 마그마 바다에 해당하는 압력에서 성공 여부를 예측하기에 충분하다. 또한 윤곽 적당히 약간 siderophile 소자 (MSE와 각각 SSE) 멀티 앤빌 장치를 사용하여 분할을 결정하는 데 사용되는 일반적인 접근법이다. 높은 압력 HSES의 포함이없는 데이터 세트의 확장과 유사한 멀티 모루 방법을 채택 할 가능성이있다. 옷에테르, 이러한 절차는 코어 - 분리의 조건으로 지상파 증가의 단계 모두를 제한하는 수단을 제공한다.

<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.

규산이 낮은 F의 O 2에서 용융에서 실험에 다음 예제와 토론의 초점은 HSE의 용해도를 결정합니다. T - - 멀티 앤빌 실험 MSE 및 SSE 분할 데이터 P 제한하기 위하여 사용될 수있는 방법의 포괄적 인 예를 들어 F를 O 코어 금속 분리 2 조건을, 독자는 참조 9 칭한다 -. 11도 7B-D는 다시 표시 전형적인 실험 실행 제품에서 흩어?...

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.

실험 방법 및 높은 Siderophile 요소 흠을 억제하는 프로토콜 : 높은 압력과 온도에서 금속 규산염 분할

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

Research

Education

JoVE Journal

JoVE Core

Chemistry

Chemical Equilibrium

SCIENTISTS IN ACTION

12.4K 조회수.  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.

비디오: 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.

CO의 상 평형 측정을위한 고압 사파이어 셀<sub&gt; 2</sub&gt; / 유기농 / 물 시스템

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

연구

화학

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.

병렬 반응기 압력 및 연쇄 이동 중합 키네틱 분석을 사용하여 에틸렌 중합

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.

실내 온도에서 탄소 나노 시트의 제조

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.

의 합성을위한 프로토콜<em&gt; 직교</em&gt; -trifluoromethoxylated 아닐린 파생 상품

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.

실시간 고해상도 질량 분석에 직접 분석을 사용하여 식물 소재의 신속한 높은 처리량 종 확인

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.

고압 PX에서 단결정 회절 ^ 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 ...

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.

효율적인 고온 화학을위한 비평 형 마이크로 웨이브 플라즈마

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.

고압 액체 크로마토 그래피와 글루코 추출 및 분석을위한 간단한 방법 (HPLC)

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.

추출 및 카 테 콜 아민 신경 전달 물질과 그들의 대사 산물의 고압 액체 크로마토그래피로 분석 하는 편리한 방법

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.

미세 중력 환경에서 효율적인 태양 수소 생산을위한 실험 방법

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