This research was funded by the International Research Training Group (IRTG) &#8220;Diffusion in porous Materials&#8221;. We acknowledge the technical support from Gert Klotzsche and stimulating discussions with Steven Reichhardt, Thomas Meissner, Damian Rybicki, Tobias Herzig, Natalya Georgieva, Jonas Kohlrautz, and Michael Jurkutat.

1 설치 및 6H-SiC를 대형 콘 Boehler 형 모루의 조심 <ol><li> 장착 도구의 피스톤과 XY 판을 수정하고 휴식 공간에서 Boehler 형 받침대를 삽입합니다. </li><li> 확실히 각 받침대는 받침 플레이트에 단단히 앉아합니다. </li><li> (예 Stycast 1266)는, 자신에게 모두 좌석 앤빌 접착제, 에폭시 수지를 사용. RT에서 12 시간 또는 2 시간 동안 노에서 65 ºC위한 치료. </li><li> 충분한 모루 정렬의 경우, 백킹 플레이트를 정렬하고 두 받침대의 병렬 처리를 모니터하기 위해 M1 세트 스크류를 사용합니다. 앤빌은 비평 것으로 발견된다면, 에폭시 수지를 제거하고, 포인트 120에서 다시 시작. </li></ol> 2 가스켓 준비 <ol><li> 어닐링 구리 - 수의 칩으로 드릴 1mm 구멍 황동 가이드 핀 (% w 구리 (98)는, 2 중량 %, 0.5 mm의 두께로한다). </li><li> GUID의 역할을하는, 앤빌 따라 분포되는 구멍으로 세 5mm 1 mm 직경의 비 절연 된 구리 와이어의 긴 조각을 삽입구리가 되실 가스켓 전자 핀. </li><li> 가이드 핀과 세포체 사이의 적절한 접지를 확인합니다. 통상적으로, 약 0.1 Ω의 DC 저항은 바람직하다. 전도성 실버 소량의 응용 프로그램을 개선 할 수 있습니다. </li><li> 모이 사 나이트 모루 위에 구리가 되실 칩을 삽입하고 셀을 닫습니다. </li><li> 유압 프레스를 사용하여 극대화 된 작업의 안정성을 위해 culet 직경의 약 8 일에 가스켓 압력을. 마이크로 미터 캘리퍼스를 사용하여 들여 쓰기의 실제 두께를 모니터링합니다. </li><li> 들여 쓰기의 중심에 적절한 직경 (culet 직경의 ½)의 구멍을 뚫습니다. </li><li> 사전 들여 가스켓으로이 채널을 개척. 채널은 마이크로 코일 18 μm의 구리 와이어를 수용 할 수있을 정도로 충분히 깊게해야한다. </li><li> 강화로에서 2 시간 3에 대한 617 K에서 제조 된 가스켓. </li></ol> 3 준비 및 마이크로 코일의 로딩 <ol><li> 1mm 구리 와이어의 조각을 사용하여피스톤의 관통 구를 통해 스레드 ㄹ. 에폭시 수지와 구리 와이어를 고정하여 단계 1.3에 따라 치료. </li><li> 마이크로 코일 원하는 직경이 송곳 (물질의 목록 참조)을 선택하고 회전 척 - 한 쌍의 죠 (jaw) 사이에 고정합니다. </li><li> 접착제 다른 쪽 끝을 잡고, 척 턱 위에 18 μm의 구리 와이어의 한쪽 끝 (SCB에서 예를 들면, 니스와 함께, 물질의 목록 참조)와 와이어가 송곳에 코일되도록 척 턱을 돌립니다. </li><li> 마이크로 코일을 원하는 형상의 경우뿐만 아니라, 접착제에 와이어의 타단을 고정한다. </li><li> 권선 위에 소량을인가함으로써 상기 코일을 고정하기 위해 희석 된 바니쉬를 사용한다. </li><li> 테프론 테이프를 사용하여 송곳에서 신중하게 코일을 제거합니다. </li><li> 개스킷의 채널에서, 어떠한 첨가물없이, 일부 에폭시 수지 (1.3 포인트 참조) 놓는다. </li><li> 샘플 챔버 내부의 마이크로 코일을 배치하고 채널로 리드를 고정합니다. </li><li> EPOX을 치료Y 수지있어서 1.3로 진행한다. </li><li> 열선에 마이크로 코일과 가이드 핀에 다른 하나의 리드를 납땜. </li><li> 각 접합의 상단에 약간은 도전성 페이스트를 추가합니다. 일반적으로 치료하는 것은 어떤 분 정도 소요됩니다. </li><li> 에폭시 수지의 양쪽과 소량의 접합부를 밀봉. </li><li> 130 단계에있어서, 에폭시 경화. </li><li> 이제, 각 단계 후에 코일의 DC 저항을 확인. </li><li> 마이크로 코일의 샘플을 놓습니다. 불필요한 신체 접촉은 코일을 파괴 할 수 있음을주의하십시오. </li><li> 압력 보정을위한 시료에 미세하게 분쇄 루비 파우더를 추가합니다. </li><li> 마지막으로, 적절한 압력 매체와 샘플 챔버 홍수. 9 GPa로까지 거의 - 수압 조건을 보장하기 위해 파라핀 오일을 사용합니다. </li><li> 조심스럽게 셀을 닫습니다. </li></ol> (4) 적용 및 압력 모니터링 <ol><li> 처음에는 약간 M3 육각 접시 머리 나사를 조입니다. </li><li> 가압은 바이스에 셀을 수정합니다. 이제, 조마주 보는 두 개의 나사 페어. </li><li> 적절한 셀 홀더에 압력 셀을 놓습니다. </li><li> 레이저 빔이 샘플 챔버에 도달 할 수 있도록 셀의 위치를​​ 조정한다. </li><li> 레이저 빔에 루비 파우더 초점을 미세 조정 테이블을 사용합니다. </li><li> 분광계 해당 소프트웨어를 사용하여 루비 광 발광 스펙트럼을 모니터한다. </li><li> 루비 R1과 R2 라인의 관찰 된 스펙트럼 변화에서 샘플 공동의 실제 압력의 압축을 풉니 다. </li><li> NMR 측정이 시작되기 전에 최소 12 시간 동안 세포를 가압 평형. </li></ol> 5 수행 NMR 실험 <ol><li> 일반적인 NMR 프로브에 압력 셀을 탑재합니다. 기계 작업장에서 적절한 셀 홀더 제조. </li><li> 프로브에 열선을 납땜. 셀과 프로브 사이의 적절한 전기적 접촉을 확인합니다. </li><li> 이제 표준 NMR 실험을 수행합니다. 마이크로 코일 VER 사실에주의를 집중인가 고주파 전력에 민감한 Y. </li></ol>

<ol>
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The authors have nothing to disclose.

기가 파스칼 압력에서 NMR을 수행 할 수있는 새로운 유망 방법에 대하여 설명 하였다. 이 방법으로 인해 우수한 감도와 해상도로 NMR 실험의 폭 넓은 다양한 문을 엽니 다. 그럼에도 불구하고, 프로토콜 절에 설명 된 여러 단계의 실험 결과에 결정적이다. 특히, 마이크로 코일의 준비 및 구리 되실 가스켓에서의 고정이 매우 어렵고 경험이 필요합니다. 다음에, 몇 가지 중요한 팁은 기술의 최초의 성?...

지난 세기의 시작 부분에서 높은 수압 압력에서 응축 물질의 퍼시 브리지 먼의 특징 실험 이후, 고압 물리학의 분야는 급속 한 발전했다. 흥미로운 현상의 많은 여러 GPa로 (2)의 압력에 따라 발생하는 것으로 알려져있다. 또한, 고압으로 응축 물질 시스템의 응답은 우리에게 자신의 전자 지상과 흥분 상태 3,4에 대해 많은 것을 가르쳤다. 불행하게도, 기가 파스칼의 압력에서 응축 물질의 전기적 성질의 조사 기술은 X 선이나 방법 5를 선도 DC 저항 측정으로 드물다. 특히, 전자 스핀 (ESR) 또는 핵 자기 공명 (NMR) 실험으로 전자 또는 핵 자기 모멘트의 검출은 하나의 신호를 검색 할 필요 전형적인 고압 앤빌 세포에서 구현하는 것은 거의 불가능할 수밖에 작은 Volume 받침대 및 밀봉 가스켓에 안치. 몇몇 그룹이 복소 배열을 사용하여이 문제를 해결하는 시도 등이 분할 한 쌍의 무선 주파수 (RF) 코일은 받침대 (6)의 측면을 따라 감겨, 단일 또는 이중 루프 머리 핀 공진기 7,8; . 예컨대 1과 핵 γ - 또는 RF 픽업 코일 (9),도 1 참조 심지어 분할 레늄 가스켓 불행히도, 그러한 접근법은 여전히 대형까지 실험 응용을 제한, 낮은 신호 대 잡음비 (SNR)을 앓고 H 10. 15 - 관심있는 독자는 다른 고압 공진 탱크 회로 실험 11 지칭 될 수있다. Pravica 및 Silvera 16 보고서 수소의 오르토 - 파라 변환을 공부 12.8 GPa로와 NMR에 대한 앤빌 셀에 달성 된 가장 높은 압력. NMR을 적용에 큰 관심과 함께양자 고체의 특성을 연구하기 위해, 우리 그룹뿐만 아니라, 높은 압력에서 사용할 수 NMR 데에 관심이 있었다. 마지막으로, 2009 년에이를 공명 무선 주파수 (RF) 마이크로 코일 (17)을 둘러싸는 샘플 고압 캐비티에 직접 배치되는 경우 고감도 앤빌 셀 NMR 정말로 가능하다는 것을 입증 할 수 있었다. 이러한 접근법에서, NMR 감도의 분말 샘플에 대해 17 O NMR 예 더욱 도전 NMR 실험을 가능하게, (RF 코일의 계수를 채우기에 주로 기인 극적인 증가) 수십배에 의해 향상된다 최대 7 GPa로 (18)에서 고온 초전도체. 이들 재료의 초전도 크게 압력의인가에 의해 증폭 될 수 있으며, 프로세스에 지배 근본적인 통찰력을 약속 로컬 전자 탐침이 프로세스를 수행하는 것이 가능하다. 무엇인지 고압 NMR의 힘에 대한 또 다른 예는 등장 believED 루틴 퍼런 실험으로 : - 단순 알루미늄 금속을 도입 새로운 앤빌 셀 NMR을 테스트하기 위해, 잘 알려진 물질 중 하나를 측정 하였다. 압력이 증가함에 따라, 하나는 자유 전자 시스템에 대해 무엇을 기대에서 NMR 변화의 예기치 않은 편차가 발견되었다. 증가 된 압력에 따라 또한, 실험을 반복, 새로운 결과가 참으로 신뢰할 수있는 것으로 나타났다. 컴퓨팅 파워가 낮을 때 마지막 밴드 구조 계산으로는, 결과 년전 계산에 의해 검출 될 수없는 알루미늄 페르미 표면의 위상 전이의 표현 인 것으로 밝혀졌다. 주변 조건에 대한 연구 결과의 외삽은 거의 모든 곳에서 사용이 금속의 성질이 특별한 전자 조건에 의해 영향을받는 것으로 나타났다. 서로 다른 응용 프로그램의 수를 추구하기 위해 특별히 디자인 된 앤빌 셀 (이전 셀은 Cavend에서 수입했다NMR을 위해 개조 틱 연​​구소와) 개발되었다. 현재 사용되는 조립식 섀시는 800 μM의 culet 6H-SiC를 앤빌의 쌍을 사용하여 25 GPa의 최대 압력에 도달 할 수있다. NMR 실험은 성공적 지금까지, 10.1 GPa로까지 수행 하였다. 이 새로운 셀 NMR 성능은 19 우수한 것으로 나타났다. 주성분은 티타늄 - 알루미늄 (6) -Vanadium (4)에 대한 (800)의 항복 강도가 20 MPa로 제공 여분 낮은 격자 간 레벨 (등급 23)와. 인해 비 자기 특성 (자기 자화율 χ 약 5 ppm의 경우)는 앤빌 셀 섀시의 적절한 소재이다. 도입 된 세포 (모든 조립식 앤빌 셀 설계의 개요를 그림 2 참조)의 전체 크기는 일반 표준 구멍 NMR 자석에 들어갈 정도로 작다. 높이 만 20mm, 직경 17mm 인 작은 디자인, LAC-TM1은 또한 전형적인 작은 냉간 구멍 자석 (30mm 구멍 직경)에 적합합니다. L저자 설계된 최신 섀시 인 AC-TM2는 (내부 압력의 매끄러운 제어에 부착 청사진을 허용 압력 구동 메커니즘 (셀 섀시와 같은 합금으로 만들어진) 사 M4 육각 카운터 싱크 볼트를 사용 보충 절). 통상적으로, 다이아몬드 앤빌 100 GPa의 전술의 최고 압력을 생성하기 위해 사용된다. 쑤 마오 21-23 moissanite의 앤빌은 약 60 GPa의 압력의 최대 고압 연구 비용 효율적인 대안을 제공하는 것을 보여 주었다. 따라서, 모이 사 나이트 모루는 도입 GPa의 NMR 방법을 사용 하였다. 가장 좋은 결과는 찰스 &amp; Colvard의 모루 부서의 사용자 정의 대형 콘 6H-SiC를 모루 달성 하였다. 그 세포로, 1​​0.1 GPa의 최대 압력에 대해, 800 μM의 culet 앤빌의 사용은 아주 좋은 NMR 감도가 낮아 밝혀졌다. 비교를 위해, Lee 등은 알. 1 H NM 1의 SNR을보고도입 마이크로 코일 방식의 SNR에도 약간 낮은 자기장에서의 7.2 부피에 대해 25의 값을 보였다 수돗물 R,. 현대 물질의 물리와 화학에 흥미 진진한 새로운 통찰력을 약속 많은 응용 프로그램을 추구 할 수 고감도 세포와 모루 NMR의 일에이 새로운 접근 방식. 하나는 작은 크기 culet 요구 훨씬 높은 압력 관심 경우에는 항상 같은 감도 및 해상도는 궁극적으로, 특히, NMR의 적용을 제한한다. 그런 다음, 하나는 더 작은 RF 코​​일과 셀 설계를 최적화뿐만 아니라, 핵 분극을 증가시키기위한 방법에 대해 생각뿐만 아니라 있습니다.

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high-sensitivity nuclear magnetic resonance at giga-pascal pressures: a new tool for probing electronic and chemical properties of condensed matter under extreme conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

그림 3은 일반적인 NMR 프로브 상에 완전히 조립 된 압력 셀, 배선 및 설치가 같이 방법을 보여줍니다. 다음에 몇 가지 실험 이점과 도입 기술의 한계에 대한 광범위한 개요를 수집하는 독자를 활성화해야하는 검토 될 것이다. <img alt="그림 1" src="/files/ftp_upload/52243/52243fig1highres.jpg" /> 그림 고압 NMR에 대한 다양한 접근 방법 1 :</s...

Watch this Scientific Journal Video about High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extr

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

극한의 상황에서도 응집 물질의 전자 화학적 특성을 프로빙을위한 새로운 도구 : 기가 파스칼의 압력에서 고감도 핵 자기 공명

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

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Principles of Nuclear Magnetic Resonance

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11.5K 조회수.  University of Leipzig. Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

비디오: High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Hyperpolarized Xenon for NMR and MRI Applications

Nuclear magnetic resonance (NMR) spectroscopy and imaging (MRI) suffer from intrinsic low sensitivity because even strong external magnetic fields of ~10 T generate only a small detectable net-magnetization of the sample at room temperature 1. Hence, most NMR and MRI applications rely on the detection of molecules at relative high concentration (e.g., water for imaging of biological tissue) or require excessive acquisition times. This limits our ability to exploit the very useful molecular specificity of NMR signals for many biochemical and medical applications. However, novel approaches have emerged in the past few years: Manipulation of the detected spin species prior to detection inside the NMR/MRI magnet can dramatically increase the magnetization and therefore allows detection of molecules at much lower concentration 2.
Here, we present a method for polarization of a xenon gas mixture (2-5% Xe, 10% N2, He balance) in a compact setup with a ca. 16000-fold signal enhancement. Modern line-narrowed diode lasers allow efficient polarization 7 and immediate use of gas mixture even if the noble gas is not separated from the other components. The SEOP apparatus is explained and determination of the achieved spin polarization is demonstrated for performance control of the method.
The hyperpolarized gas can be used for void space imaging, including gas flow imaging or diffusion studies at the interfaces with other materials 8,9. Moreover, the Xe NMR signal is extremely sensitive to its molecular environment 6. This enables the option to use it as an NMR/MRI contrast agent when dissolved in aqueous solution with functionalized molecular hosts that temporarily trap the gas 10,11. Direct detection and high-sensitivity indirect detection of such constructs is demonstrated in both spectroscopic and imaging mode.

The production of hyperpolarized xenon by means of spin exchange optical pumping (SEOP) is described. This method yields a ~10000-fold enhancement of the nuclear spin polarization of Xe-129 and has applications in nuclear magnetic resonance spectroscopy and imaging. Examples of gas phase and solution state experiments are given.

NMR과 MRI 응용 프로그램 용 Hyperpolarized 지논

Nuclear magnetic resonance (NMR) spectroscopy and imaging (MRI) suffer from intrinsic low sensitivity because even strong external magnetic fields of ~10 ...

연구

공학

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.

극단적 인 압력과 온도에서 합성 부위 회절

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

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.

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 ...

환경과학

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 ...

화학

High-Pressure NMR Experiments for Detecting Protein Low-Lying Conformational States

High-pressure is a well-known perturbation method that can be used to destabilize globular proteins and dissociate protein complexes in a reversible manner. Hydrostatic pressure drives thermodynamical equilibria toward the state(s) with the lower molar volume. Increasing pressure offers, therefore, the opportunities to finely tune the stability of globular proteins and the oligomerization equilibria of protein complexes. High-pressure NMR experiments allow a detailed characterization of the factors governing the stability of globular proteins, their folding mechanisms, and oligomerization mechanisms by combining the fine stability tuning ability of pressure perturbation and the site resolution offered by solution NMR spectroscopy. Here we present a protocol to probe the local folding stability of a protein via a set of 2D 1H-15N experiments recorded from 1 bar to 2.5 kbar. The steps required for the acquisition and analysis of such experiments are illustrated with data acquired on the RRM2 domain of hnRNPA1.

We provide a detailed description of the steps required to assemble a high-pressure cell, set up and record high-pressure NMR experiments, and finally analyze both peak intensity and chemical shift changes under pressure. These experiments can provide valuable insights into the folding pathways and structural stability of proteins.

High-pressure is a well-known perturbation method that can be used to destabilize globular proteins and dissociate protein complexes in a reversible ...

생화학

An Externally-Heated Diamond Anvil Cell for Synthesis and Single-Crystal Elasticity Determination of Ice-VII at High Pressure-Temperature Conditions

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in Earth&#8217;s and planetary interiors. Here we describe the design and fabrication of the EHDAC assemblies and accessories, including ring resistive heaters, thermal and electrical insulating layers, thermocouple placement, as well as the experimental protocol for preparing the EHDAC using these parts. The EHDAC can be routinely used to generate megabar pressures and up to 900 K temperatures in open air, and potentially higher temperatures up to ~1200 K with a protective atmosphere (i.e., Ar mixed with 1% H2). Compared with a laser-heating method for reaching temperatures typically &#62;1100 K, external heating can be easily implemented and provide a more stable temperature at &#8804;900 K and less temperature gradients to the sample. We showcased the application of the EHDAC for synthesis of single crystal ice-VII and studied its single-crystal elastic properties using synchrotron-based X-ray diffraction and Brillouin scattering at simultaneously high-pressure high-temperature conditions.

This work focuses on the standard protocol for preparing the externally-heated diamond anvil cell (EHDAC) for generating high-pressure and high-temperature (HPHT) conditions. The EHDAC is employed to investigate materials in Earth and planetary interiors under extreme conditions, which can be also used in solid state physics and chemistry studies.

고압 온도 조건에서 얼음 VII의 합성 및 단결정 탄성 측정을 위한 외부 가열 다이아몬드 모루 셀

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in ...

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Nuclear magnetic resonance (NMR) spectroscopy represents an important technique to understand the structure and bonding environments of molecules. There exists a drive to characterize materials under conditions relevant to the chemical process of interest. To address this, in situ high-temperature, high-pressure MAS NMR methods have been developed to enable the observation of chemical interactions over a range of pressures (vacuum to several hundred bar) and temperatures (well below 0 &#176;C to 250 &#176;C). Further, the chemical identity of the samples can be comprised of solids, liquids, and gases or mixtures of the three. The method incorporates all-zirconia NMR rotors (sample holder for MAS NMR) which can be sealed using a threaded cap to compress an O-ring. This rotor exhibits great chemical resistance, temperature compatibility, low NMR background, and can withstand high pressures. These combined factors enable it to be utilized in a wide range of system combinations, which in turn permit its use in diverse fields as carbon sequestration, catalysis, material science, geochemistry, and biology. The flexibility of this technique makes it an attractive option for scientists from numerous disciplines.

The molecular structures and dynamics of solids, liquids, gases, and mixtures are of critical interest to diverse scientific fields. High-temperature, high-pressure in situ MAS NMR enables detection of the chemical environment of constituents in mixed phase systems under tightly controlled chemical environments.

Nuclear magnetic resonance (NMR) spectroscopy represents an important technique to understand the structure and bonding environments of molecules. There ...

High-Resolution Studies of Proteins in Natural Membranes by Solid-State NMR

Membrane proteins are vital for cell function and thus represent important drug targets. Solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy offers a unique access to probe the structure and dynamics of such proteins in biological membranes of increasing complexity. Here, we present modern solid-state NMR spectroscopy as a tool to study structure and dynamics of proteins in natural lipid membranes and at atomic scale. Such spectroscopic studies profit from the use of high-sensitivity ssNMR methods, i.e., proton-(1H)-detected ssNMR and DNP (Dynamic Nuclear Polarization) supported ssNMR. Using bacterial outer membrane beta-barrel protein BamA and the ion channel KcsA, we present methods to prepare isotope-labeled membrane proteins and to derive structural and motional information by ssNMR.

This work details robust basic routines on how to prepare isotope-labeled membrane protein samples and analyze them at high-resolution with modern solid-state NMR spectroscopy methods.

Membrane proteins are vital for cell function and thus represent important drug targets. Solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy ...

High-Speed Magnetic Tweezers for Nanomechanical Measurements on Force-Sensitive Elements

Single-molecule magnetic tweezers (MTs) have served as powerful tools to forcefully interrogate biomolecules, such as nucleic acids and proteins, and are therefore poised to be useful in the field of mechanobiology. Since the method commonly relies on image-based tracking of magnetic beads, the speed limit in recording and analyzing images, as well as the thermal fluctuations of the beads, has long hampered its application in observing small and fast structural changes in target molecules. This article describes detailed methods for the construction and operation of a high-resolution MT setup that can resolve nanoscale, millisecond dynamics of biomolecules and their complexes. As application examples, experiments with DNA hairpins and SNARE complexes (membrane-fusion machinery) are demonstrated, focusing on how their transient states and transitions can be detected in the presence of piconewton-scale forces. We expect that high-speed MTs will continue to enable high-precision nanomechanical measurements on molecules that sense, transmit, and generate forces in cells, and thereby deepen our molecular-level understanding of mechanobiology.

Here, we describe a high-speed magnetic tweezer setup that performs nanomechanical measurements on force-sensitive biomolecules at the maximum rate of 1.2 kHz. We introduce its application to DNA hairpins and SNARE complexes as model systems, but it will be also applicable to other molecules involved in mechanobiological events.

힘에 민감한 요소에 대한 나노 역학 측정을 위한 고속 자기 핀셋

Single-molecule magnetic tweezers (MTs) have served as powerful tools to forcefully interrogate biomolecules, such as nucleic acids and proteins, and are ...

Cryogenic Sample Loading into a Magic Angle Spinning Nuclear Magnetic Resonance Spectrometer that Preserves Cellular Viability

Dynamic nuclear polarization (DNP) can dramatically increase the sensitivity of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. These sensitivity gains increase as temperatures decrease and are large enough to enable the study of molecules at very low concentrations at the operating temperatures (~100 K) of most commercial DNP-equipped NMR spectrometers. This leads to the possibility of in-cell structural biology on cryopreserved cells for macromolecules at their endogenous levels in their native environments. However, the freezing rates required for cellular cryopreservation are exceeded during typical sample handling for DNP MAS NMR and this results in loss of cellular integrity and viability. This article describes a detailed protocol for the preparation and cryogenic transfer of a frozen sample of mammalian cells into a MAS NMR spectrometer.

Presented here is a protocol for cryogenic transfer of frozen samples into the dynamic nuclear polarization (DNP) magic angle spinning (MAS) nuclear magnetic resonance (NMR) probe. The protocol includes directions for rotor storage prior to the experiment and directions for viability measurements before and after the experiment.

셀룰러 생존력을 보존하는 마법의 각도 회전 핵 자기 공명 분광기에 극저온 샘플 로딩

Dynamic nuclear polarization (DNP) can dramatically increase the sensitivity of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. ...