이 작품은 협업 프로젝트 BOR4STORE (부여 계약 번호 303428) 및 인프라 프로그램 H2FC (보조금 협정 제 FP7-284522)에서 유럽의 연료 전지 및 Hydruogen 공동 Undertaking에 의해 지원되었다.

1. 장치 <ol><li> 가스 공급기, 진공 시스템, 센서 (온도 및 압력), 및 (욕에 침지 될 수있는) 샘플 환경 : 고압 가스 배관으로 연결된 네 개의 주요 구성 요소로 이루어진 기본 초 임계 건조 (SCD) 장치를 사용. 건축 고품질 스테인리스 밸브, 피팅, 및 튜브 인 것을 확인, 80-300 K. 사이의 온도 범위에서 적어도 10 MPa의 압력이 정격 참고 : 회로도는 그림 1에 표시됩니다. </li><li> 질소 SCD (NSCD) 트리트먼트, 가스 공급 연구 순도는 0-10 MPa의 출구 사이의 압력 제어를위한 압력 조절기를 장착 (&gt; 99.999 %) 질소 가스가 있음을 보장한다. 장치 50 L 병 (20 MPa로)를 연결하고 사용 전에 순수한 질소를 여러 번으로 시스템을 퍼지. </li><li> 진공 시스템은 0.1Pa로 &lt;까지 진공 압력을 달성 할 수 있고, 장치에 연결되어 있는지 확인미세 제어 니들 밸브. 바람직하게는, 직렬로 배치 된 오일 프리 러핑 펌프와 분자 드래그 터보 펌프를 사용한다. </li><li> SCD 치료 동안에 압력의 정확한 측정을위한 적어도 두 개의 압력 센서를 사용하여 측정 및 진공 고압 센서 저압 센서가 0.1 내지 7 파 사이 총 측정 압력 범위를 달성했다. </li><li> 전형적인 SCD 치료를 수행하기 위해 필요한 최소한의 정확성을 위해 적어도 두 온도 센서를 사용하는 센서를 샘플 및 77-300 K 사이의 정확한 측정을위한 기본 가스 투약 폴드 내의 센서와 열 접촉 (예를 들면, K 형 열전대) . </li><li> 샘플 홀더는 처리에 필요한 시료의 양을 포함하는 적당한 내부 체적을 가지며, 스테인리스 강으로 제작되어 있는지 확인한다. 참고 : 목욕과 열 접촉에 길게 원통형 디자인 에이즈. </li><li> 샘플 용기를 닫 피팅 appropr 있는지 확인높은 압력과 반복 사용 (예를 들어,은 Swagelok VCR)에 늦는. 욕조에 샘플 홀더의 완전한 몰입을위한 튜브의 적절한 길이 (딥 튜브)를 통해 외부 환경으로부터 격리를위한 밸브 샘플 용기 볼륨을 연결합니다. </li></ol><img alt="그림 1" src="/files/ftp_upload/52817/52817fig1.jpg" /> . 욕에서 시료의 침수 후 상온 (B)에서 (A) :도 1 초 임계 건조 질소 (NSCD) 장치 전형적인 실험실에서 사용하기위한 장치의 단순화 된 NSCD 개략도. 이 연구에서 기술 된 프로세스에 대한 가스 공급을 질소이지만, 이러한 일반적인 장치는 CO 2 등의 온도와 압력의 범위 내에서 실질적 누워 임계점 다른 SCD 유체로 일반화된다. 구성 요소는 제와 일관성을 위해 표시되어 있습니다프로토콜은 여기에 설명 된 전자. <a href="https://www.jove.com/files/ftp_upload/52817/52817fig1highres.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> 2. 준비 <ol><li> 샘플의 하중 0.2-0.5 g (γ-마그네슘 (BH 4) 2, 분말 형태의 습식 화학 합성 표준 건조 방법에 따라) 예컨대 아르곤 글로브 박스로서 전형적으로 불활성 분위기에서 적절한 조건하에 시료 홀더로, 아래 또는 주위 온도. 필터 가스켓 샘플 홀더 (피팅 F2)를 닫고 밸브 (밸브 V4)를 닫습니다. 장치에 샘플 홀더를 전송하고 (피팅 F1)를 연결합니다. </li><li> (V2)를 통해 진공 청소기 대피 투여 매니 폴드를 엽니 다. 열기 V3 및 피난. (V1)을 통해 질소와 장치를 제거하고 (V2)를 통해 대피. 오픈 V4는 시스템 (&lt;0.1 ​​PA)의 최소 압력에 도달하기까지 24 시간 동안 RT에서 샘플을 피난. </li><li> 샘플 목욕을 설치 (참조 <stronG&gt; 샘플 홀더 주위에 그림 2). 가위 리프트, 또는 유사한 메커니즘에 위치로 목욕을 제기하여이 작업을 수행합니다. </li><li> 110 K의 (단계 3.1 참조, T의 L) 원하는 미래 액체 온도로 히터를 설정하고 온도가 평형을 때까지 장치를 철수하는 것을 계속한다. </li></ol><img alt="그림 2" src="/files/ftp_upload/52817/52817fig2.jpg" /> 그림 2. 극저온 전기로 샘플 목욕. (왼쪽) 개략도 및 저온 유지 열 목욕 환경의 사진 (오른쪽), nscd를 처리하는 동안 샘플 홀더를 포함하는 측정 및 77-298 케이 사이의 시료 온도 제어를 허용하기위한 적절한 <a href="https://www.jove.com/files/ftp_upload/52817/52817fig2highres.jpg" target="_blank">하세요 이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> 3. 초 임계 질소 노출 <ol&gt; <li> γ - 마그네슘 (BH 4) 2, (이 프로토콜에서 시연의 주제)의 NSCD 처리를 위해이 적당한 액체 용매 밀도에 해당하는 110 케이의 액체 온도 (T의 L)을 선택 (~ 0.6 g을 ml의 -1) ; 다른 nscd를 처리 공정에이 프로토콜의 응용 프로그램에 대한 필요에 따라 조정합니다 (아래 참고 참조). </li><li> V2를 닫아 진공 시스템을 닫습니다. 압력이 상태도의 액체 영역으로 증가 할 수 있도록, 서서히 개방 V1을 스로틀 링. 2 MPa의와 T L에서 시스템을 평형. </li><li> 4 시간 동안 액체 N 2의 샘플을 만끽 해보세요. </li><li> 램프 ≤2 K 분 -1 150 (K)에 히터를 설정합니다. 압력 (이 P 최대가 MPa의 ≥10해야한다) 장치의 최대 정격 압력보다 더 이상 증가하지 않습니다 허용; 필요한 경우라면, V2를 통해 진공하는 초과 압력을 벤트. P 최대 150 K.에 시스템을 평형 </li><li> SUP의 샘플을 적시1 시간 동안 ercritical N 2. </li></ol><img alt="그림 3" src="/files/ftp_upload/52817/52817fig3.jpg" /> 도 3 질소의 위상 다이어그램. 유체 밀도 (선형 스케일에 도시) 질소의 상세한 상태도 Refprop (상태의 개질 웹은-베네딕트 - 루빈 방정식)을 사용하여 계산된다. 일정한 밀도의 41 다양 라인 나타낸다 보라색. 고상 경계와 전이 비등 라인 빨간색으로 표시되어있다. 파란색 선은 N 2를 사용하여 건조 또는 추출 처리를 위해 관련 상태도의 영역의 경계를 나타냅니다. <a href="https://www.jove.com/files/ftp_upload/52817/52817fig3highres.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> 다른 물질이 프로토콜의 응용 프로그램에 대한 적절한 nscd를 처리 schem을 설정 참고 :표적 종의 효과적인 용 매화하기 위해 필요한 조건을 선택하여 E. 도 3에 도시 된 N (2)의 상태도를 참조. 액상 유체 높은 밀도를 달성하기 위해 (예를 들어, g는 0.8-1 ml의 -1), 적당한 액체 밀도 80-90 K.의 T의 L을 선택 (예를 들어, 0.6-0.8 G ml의 -1), 필요할 수 있습니다 90-115 케이 시행 착오 방식의 T는 L을 선택합니다. 4. 초 임계 질소 출시 <ol><li> 조심스럽게 V2을 스로틀 압력은 가능한 한 느리게 감소시킴으로써 진공 시스템 균열. 반복적 12-24 hr의 대략적인 시간 범위에서 고 진공 (&lt;0.1 ​​PA)에 점진적 감소를 달성하기 위해 필요에 따라 더 높은 속도로 진공 시스템 균열. </li><li> 완전히 샘플을 대피 샘플 목욕 및 완전 개방 (V2)를 제거합니다. RT 및 고진공 (&lt;0.1 ​​PA)에서 평형. </li><li> D로, 1-24 시간 동안 RT와 &lt;0.1 ​​아빠의 샘플을 드가esired. </li></ol> 5. 사후 처리 <ol><li> 닫기 밸브 V3 및 V4, 그리고 (F1 피팅) 장치로부터 샘플 홀더를 제거합니다. </li><li> 예컨대 아르곤 충진 글로브 박스와 같은 처리를 위해 불활성 환경에 샘플 홀더를 이동. 아래의 주위 온도 또​​는 밀봉 된 용기에 시료 (F2 피팅) 홀더와 상점에서 샘플을 제거합니다. </li></ol>

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저자가 공개하는 게 없다.

아마도 상대적으로 낮은 임계 온도 (126 K)로 인해, N (2)는 역사적으로 효과적인 SCD 용매로서 간과하고있다. 이전의보고에서, 3,17,42,43은 만 제외 (인해 상태도의이 영역에서의 낮은 유체 밀도 또는 단지 적당한 매화 전력을 나타내는 주변, 이상의 온도 처리의 맥락에서 언급 한 내용 매우 높은 압력 (43))에서. 초 임계 용매로서 N (2)의 실용성을 실현하는데 핵심 단계?...

건조 초 임계 유체 추출 (SFE) 및 (SCD) 방법이 아니라, 특히 식품 및 석유 산업에서, 실제 응용의 넓은 범위에서 설정뿐만 아니라, 화학 합성, 분석 및 재료 처리. 1-6 건조 사용되는 또는 임계점 위의 조건에서 추출 매체들은 더 빠르고, 깨끗하고 효율적인 전통 (액체) 기법에 비해, 높은 작동 조건의 약간의 조정에 의해 유체의 매화 전원에 대하여 동조되는 추가적인 장점을 갖는다 . 3,7 간단한 SCD 방법은 세 가지 기본 단계로 구성되어 있습니다. 첫 번째 단계는 액체에 적절하게 선택된 SCD 액에 대상 불순 화합물을 함유하는 출발 고체 (혹은 액체) 물질에 노출되어 높은 밀도가 높은 (어쩌면 선택성에 대응 (또는 거의 액체 초임)의 위상, 대상 종에 대한 7) 용매의 전원을 켭니다. 티그 두 번째 단계는 가열 유체와 용해 목표 종 분리를 초래할 수 위상 경계가 통과하지 않도록, 밀폐 용기에 선택된 SCD 유체의 임계점 위의 압축 시스템이다. 마지막 단계는 천천히 위상 경계 또는 도중에 어떠한 해로운 표면 장력 효과가 발생하지 않고, 다시 탈출 대상 종을 포함하는 액체 용액을 허용 임계 온도 이상의 온도에서 진공 SCD 유체의 압력을 감압한다. 출발 물질은 표적 종 고갈 채로 필요하다면 반복 치료를 실시 할 수있다. 초 임계 유체 추출의 경우, 대상 용질 종 목적 생성물이고, 다른 경우에는 더욱 사용하기위한 용액으로부터. -8,9- 수집, 건조 또는 정제 된 출발 물질이 목적 생성물이며, 추출 된 불순물은 폐기된다. 후자의 시나리오, 본 명세서SCD 접근으로서, 높은 표면적, 진공 하에서 기존의 열처리 방법은 많은 경우에 기공을 비운에 충분하지 않은 유기 금속 틀 (MOFs와) 같은 미세 다공성 물질의 전처리에 대한 효율적인 전략으로 밝혀졌다 모든 원치 않는 손님, 또는 기공 붕괴 초래한다. (10) 이산화탄소 SCD (CSCD) 처리는 지금까지 1,000 %에 치료 물질을 통해 질소가 접촉 할 수있는 표면 영역의 증가로 이어지는으로 MOFs, 11 일과 후 합성 과정 12 이러한 촉매 활성 등의 개선. (13) 다른 주목할만한 초 임계 유체 응용 화학 반응을위한 광범위하게 조정할 수있는 매체로하고, 14 ~ 16 초 임계 유체 크로마토 그래피 (SCFC) 6,17,18 및 에어로젤과 첨단 복합 재료의 합성. 19- (22) 애플리케이션을 건조, SCD 유체는 두 가지 기준을 기반으로 선택된다 : a) 동작의 근접성중요한 포인트는 (편의를 위해 에너지 비용이나 공정의 복잡성 감소시키는)을 주위 조건하는 표적 종에 대해서와 b)의 용 매화 전원. 이산화탄소 (CO 2)가, 비 독성, 불연성 및 저렴한 때문에 많은 응용에서 편리한 SCD 유체 입증하고 있으며, 그 근처에 액체 일반적인 유기 표적 종의 수를 향해 높은 용 매화 능력을 나타내도록 조정될 수있다 . 1-3,7-9 다른 일반적인 초 임계 용매 (또는 공용 매) (&lt;10 MPa로 압력과 273-323 K의 온도에서) 상태는 물 (그 주위 온도 및 초 임계 상태 사이의 용매 특성의 놀라운 범위에 걸쳐 포함 극성 (양성 자성 및 비 양성 자성) 비극성에 및 주변 조건에 비교적 가까운 임계점을 갖는로부터 스펙트럼을 커버 (23)), 아세톤, 에틸렌, 메탄올, 에탄올, 및 에탄. 이산화탄소가 사용될까지 가장 흔한 SCD 유체가있다. CSCD 확립 방법에있어서, 반응성출발 물질이없는 방청 인자의 CO 2 임계점 부근의 온도에서 매우 약하게 반응성 때문이다. 그러나, 가열 하에서 그들의 (아마도 의도적 맞춤) 불안정성에 부가 물 또는 이산화탄소의 존재 하에서 강한 반응성 소위 복합 하이드 라이드 (예를 들어, 알라 네이트 및 보로 하이드 라이드) 처리에서 본 독특한 도전 재료로서 특정 부류 . 24-26은 또한 나노 구조 및 / 또는 다공성 31-33 품종에 따라서도 큰 국제 고밀도 수소 저장 화합물, 27-30 등의 재료에 대한 관심이있다. 반응성, 불안정 및 나노 물질의 효율적인 정제를 위해, SCD 방법은 좁은 공동으로 침투에 적합한 작은 분자 직경을 가지고 있으며, 또한 향해 높은 용 매화 능력을 갖는다. 34 SCD 유체가 사용되어야 유망한 전략 아르 타겟 불순물 WHI르는 출발 물질 자체 향해 반응성 나머지. 여기서, 예컨대 추출, 특히 건조 애플리케이션 효과적인 초 임계 유체로서 질소를 사용하는 (N 2)가 제공된다. 특정 초 임계 질소 건조 (NSCD) 방법론은 목표 종 디보 란 및 N 부틸 화합물 (비슷하지만 N 개의 뷰 테인 구체적으로 식별되지 않음)를 모두 포함 γ 상 마그네슘 보로 하이드 라이드의 정제에 대하여 설명한다. 다음 프로토콜은 쉽게 다른 초 임계 질소 건조 또는 추출 과정에 일반 연장을 수정할 수 있습니다.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Compressed Nitrogen Gas</td>
			<td>Messer Schweiz AG</td>
			<td></td>
			<td>50 L bottle, purity &#62; 99.999%, &#60;3 ppmv H2O</td>
		</tr>
		<tr>
			<td>Liquid Nitrogen</td>
			<td>Pan Gas AG</td>
			<td></td>
			<td>Bulk storage, on site</td>
		</tr>
		<tr>
			<td>Custom Supercritical Drying Apparatus</td>
			<td>Empa</td>
			<td></td>
			<td>Swagelok (compression fitting and VCR) components</td>
		</tr>
		<tr>
			<td>Custom Cryogenic Furnace Bath</td>
			<td>Empa</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Custom Labview Interface</td>
			<td>Empa</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

supercritical nitrogen processing for the purification of reactive porous materials

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. Herein, nitrogen is presented as a novel supercritical drying fluid for specialized applications such as in the processing of reactive porous materials, where carbon dioxide and other fluids are not appropriate due to their higher chemical reactivity. Nitrogen exhibits similar physical properties in the near-critical region of its phase diagram as compared to carbon dioxide: a widely tunable density up to ~1 g ml-1, modest critical pressure (3.4 MPa), and small molecular diameter of ~3.6 &#197;. The key to achieving a high solvation power of nitrogen is to apply a processing temperature in the range of 80-150 K, where the density of nitrogen is an order of magnitude higher than at similar pressures near ambient temperature. The detailed solvation properties of nitrogen, and especially its selectivity, across a wide range of common target species of extraction still require further investigation. Herein we describe a protocol for the supercritical nitrogen processing of porous magnesium borohydride.

알칼리 및 알칼리 토 금속 보로 하이드 라이드가 디보 란은 또한 때때로 탈리 가스에서 검출 된 같은 분해. 27, 29 다른 분해 생성물에 기체 수소의 큰 콘텐츠를 제공 가능한 수소 저장 물질이지만, 그 기원은 명확 선험적 아니다 ; 그들이 순수한 위상 분해 제품이지만, 또한 남은 화학 합성에서 불순물의 반응의 불순물 및 제품 일 수있다. (35), 마그네슘 보로 하이드 라이드 다공질 ?...

Watch this Scientific Journal Video about Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials at JoVE.com

Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

질소 인해 작은 분자 크기, 거의 액체, 초 임계 영역에서 고 밀도 및 화학적 불활성으로 추출 또는 건조 공정을위한 유효 임계 유체이다. 우리는 반응성, 다공성 물질의 정제 처리를 위해 초 임계 건조 질소 프로토콜을 제시한다.

반응성이 있음 다공성 물질의 정제를위한 초 임계 질소 처리

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. ...

supercritical-nitrogen-processing-for-purification-reactive-porous

Research

JoVE Journal

Chemistry

14.6K 조회수.  Empa, Swiss Federal Laboratories for Materials Science and Technology.  질소 인해 작은 분자 크기, 거의 액체, 초 임계 영역에서 고 밀도 및 화학적 불활성으로 추출 또는 건조 공정을위한 유효 임계 유체이다. 우리는 반응성, 다공성 물질의 정제 처리를 위해 초 임계 건조 질소 프로토콜을 제시한다. 

비디오: Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

Folding and Characterization of a Bio-responsive Robot from DNA Origami

The DNA nanorobot is a hollow hexagonal nanometric device, designed to open in response to specific stimuli and present cargo sequestered inside. Both stimuli and cargo can be tailored according to specific needs. Here we describe the DNA nanorobot fabrication protocol, with the use of the DNA origami technique. The procedure initiates by mixing short single-strand DNA staples into a stock mixture which is then added to a long, circular, single-strand DNA scaffold in presence of a folding buffer. A standard thermo cycler is programmed to gradually lower the mixing reaction temperature to facilitate the staples-to-scaffold annealing, which is the guiding force behind the folding of the nanorobot. Once the 60 hr folding reaction is complete, excess staples are discarded using a centrifugal filter, followed by visualization via agarose-gel electrophoresis (AGE). Finally, successful fabrication of the nanorobot is verified by transmission electron microscopy (TEM), with the use of uranyl-formate as negative stain.

DNA origami is a powerful method for fabricating precise nanoscale objects by programming the self-assembly of DNA molecules. Here we describe a protocol for the folding of a bio-responsive robot from DNA origami, its purification and negative staining for transmission electron microscopic imaging (TEM).

DNA 접기에서 바이오 응답 로봇의 폴딩 및 특성화

The DNA nanorobot is a hollow hexagonal nanometric device, designed to open in response to specific stimuli and present cargo sequestered inside. Both ...

연구

화학

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

포스 포의 향상된 농축을위한 거대 다공성 고분자 모노리스에 다공성 조정 폴리머 코팅의 제조

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

복잡한 탄화수소 행렬에 질소 함유 화합물의 온라인 분석

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Insights into the Interactions of Amino Acids and Peptides with Inorganic Materials Using Single-Molecule Force Spectroscopy

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals leads to the formation of composite materials with unique properties. In addition, the undesirable process of biofouling is initiated by the adsorption of biomolecules, mainly proteins, on surfaces. This organic layer is an adhesion layer for bacteria and allows them to interact with the surface. Understanding the fundamental forces that govern the interactions at the organic-inorganic interface is therefore important for many areas of research and could lead to the design of new materials for optical, mechanical and biomedical applications. This paper demonstrates a single-molecule force spectroscopy technique that utilizes an AFM to measure the adhesion force between either peptides or amino acids and well-defined inorganic surfaces. This technique involves a protocol for attaching the biomolecule to the AFM tip through a covalent flexible linker and single-molecule force spectroscopy measurements by atomic force microscope. In addition, an analysis of these measurements is included.

Here we present a protocol to measure the force of interactions between a well-defined inorganic surface and either peptides or amino acids by single-molecule force spectroscopy measurements using an atomic force microscope (AFM). The information obtained from the measurement is important to better understand the peptide-inorganic material interphase.

단일 분자 힘 분광학을 사용하여 무기 재료와 아미노산 및 펩타이드의 상호 작용에 대한 통찰력

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

면 대 면 모양 이방성 콜 로이드 카드뮴 칼코게나이드 Nanostructures의 연결

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three preparation methods are described: (a) the incorporation of metal salts into silica or alumina wet gels using an impregnation method; (b) the incorporation of metal salts into alumina wet gels using a co-precursor method; and (c) the addition of metal nanoparticles directly into a silica aerogel precursor mixture. The methods utilize a hydraulic hot press, which allows for rapid (&#60;6 h) supercritical extraction and results in aerogels of low density (0.10 g/mL) and high surface area (200-800 m2/g). While the work presented here focuses on the use of copper salts and copper nanoparticles, the approach can be implemented using other metal salts and nanoparticles. A protocol for testing the three-way catalytic ability of these aerogels for automotive pollution mitigation is also presented. This technique uses custom-built equipment, the Union Catalytic Testbed (UCAT), in which a simulated exhaust mixture is passed over an aerogel sample at a controlled temperature and flow rate. The system is capable of measuring the ability of the catalytic aerogels, under both oxidizing and reducing conditions, to convert CO, NO and unburned hydrocarbons (HCs) to less harmful species (CO2, H2O and N2). Example catalytic results are presented for the aerogels described.

Here we present protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms. Methods for preparing materials using copper salts and copper-containing nanoparticles are featured. Catalytic testing protocols demonstrate the effectiveness of these aerogels for three-way catalysis applications.

제조 및 급속 한 초 임계 추출 통해 준비 촉매 Aerogels의 테스트

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Deposition of Porous Sorbents on Fabric Supports

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material that can be subsequently treated by dip coating. Dip coating with a sol preparation provides a supported porous layer on the fabric. In this case, the porous layer is a porphyrin functionalized sorbent system based on a powdered material that has been demonstrated previously for the capture and conversion of phosgene. A representative coating is applied to cotton fabric at a loading level of 10 mg/g. This coating has minimal impact on water vapor transport through the fabric (93% of the support fabric rate) while significantly reducing transport of 2-chloroethyl ethyl sulfide (CEES) through the material (7% of support fabric rate). The described approaches are suitable for use with other fabrics providing amine and hydroxyl groups for modification and can be used in combination with other sol preparations to produce varying functionality.

This report details a microwave-initiated approach for deposition of porphyrin functionalized porous organosilicate sorbents on a cotton fabric and demonstrates reduction in 2-chloroethyl ethyl sulfide (CEES) transport through the fabric resulting from this treatment.

패브릭 지원에 다공성 흡수의 증 착

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its well-balanced ferroelectricity, piezoelectricity, and dielectric constant. In addition, BT does not contain any toxic elements. Therefore, it is considered to be an eco-friendly material, which has attracted considerable interest as a replacement for lead zirconate titanate (PZT). However, bulk BT loses its ferroelectricity at approximately 130 &#176;C, thus, it cannot be used at high temperatures. Because of the growing demand for high-temperature ferroelectric materials, it is important to enhance the thermal stability of ferroelectricity in BT. In previous studies, strain originating from the lattice mismatch at hetero-interfaces has been used. However, the sample preparation in this approach requires complicated and expensive physical processes, which are undesirable for practical applications.
In this study, we propose a chemical synthesis of a porous material as an alternative means of introducing strain. We synthesized a porous BT thin film using a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles were used as an organic template. Through a series of studies, we clarified that the introduction of pores had a similar effect on distorting the BT crystal lattice, to that of a hetero-interface, leading to the enhancement and stabilization of ferroelectricity. Owing to its simplicity and cost effectiveness, this fabrication process has considerable advantages over conventional methods.

Here, we present a protocol for the synthesis of porous barium titanate (BaTiO3) thin film by a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles are used as an organic template.

바 륨 다공성 타이타늄 박막 및 다공성 유도 된 긴장에 의해 Ferroelectric 단계의 열 안정화의 화학 합성

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

Synthesis and Bioconjugation of Thiol-Reactive Reagents for the Creation of Site-Selectively Modified Immunoconjugates

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. Yet maleimide-based conjugates display limited stability in vivo because the succinimidyl thioether linkage can undergo a retro-Michael reaction. This, of course, can lead to the release of the radioactive payload or its exchange with thiol-bearing biomolecules in circulation. Both of these processes can produce elevated activity concentrations in healthy organs as well as decreased activity concentrations in target tissues, resulting in reduced imaging contrast and lower therapeutic ratios. In 2018, we reported the creation of a modular, stable, and easily accessible phenyloxadiazolyl methyl sulfone reagent &#8212; dubbed &#8216;PODS&#8217; &#8212; as a platform for thiol-based bioconjugations. We have clearly demonstrated that PODS-based site-selective bioconjugations reproducibly and robustly create homogenous, well-defined, highly immunoreactive, and highly stable radioimmunoconjugates. Furthermore, preclinical experiments in murine models of colorectal cancer have shown that these site-selectively labeled radioimmunoconjugates exhibit far superior in vivo performance compared to radiolabeled antibodies synthesized via maleimide-based conjugations. In this protocol, we will describe the four-step synthesis of PODS, the creation of a bifunctional PODS-bearing variant of the ubiquitous chelator DOTA (PODS-DOTA), and the conjugation of PODS-DOTA to the HER2-targeting antibody trastuzumab.

In this protocol, we will describe the synthesis of PODS, a phenyoxadiazolyl methyl sulfone-based reagent for the site-selective attachment of cargos to the thiols of biomolecules, particularly antibodies. In addition, we will describe the synthesis and characterization of a PODS-bearing bifunctional chelator and its conjugation to a model antibody.

합성 및 Bioconjugation의 Thiol 반응 시 약 사이트에 선택적으로의 창조에 대 한 수정 Immunoconjugates

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. ...

Evaluation of Oxidative Stress in Biological Samples Using the Thiobarbituric Acid Reactive Substances Assay

Despite its limited analytical specificity and ruggedness, the thiobarbituric acid reactive substances (TBARS) assay has been widely used as a generic metric of lipid peroxidation in biological fluids. It is often considered a good indicator of the levels of oxidative stress within a biological sample, provided that the sample has been properly handled and stored. The assay involves the reaction of lipid peroxidation products, primarily malondialdehyde (MDA), with thiobarbituric acid (TBA), which leads to the formation of MDA-TBA2 adducts called TBARS. TBARS yields a red-pink color that can be measured spectrophotometrically at 532 nm. The TBARS assay is performed under acidic conditions (pH = 4) and at 95 &#176;C. Pure MDA is unstable, but these conditions allow the release of MDA from MDA bis(dimethyl acetal), which is used as the analytical standard in this method. The TBARS assay is a straightforward method that can be completed in about 2 h. Preparation of assay reagents are described in detail here. Budget-conscious researchers can use these reagents for multiple experiments at a low cost rather than buying an expensive TBARS assay kit that only permits construction of a single standard curve (and thus can only be used for one experiment). The applicability of this TBARS assay is shown in human serum, low density lipoproteins, and cell lysates. The assay is consistent and reproducible, and limits of detection of 1.1 &#956;M can be reached. Recommendations for the use and interpretation of the spectrophotometric TBARS assay are provided.

The goal of the thiobarbituric acid reactive substances assay is to assess oxidative stress in biological samples by measuring the production of lipid peroxidation products, primarily malondialdehyde, using visible wavelength spectrophotometry at 532 nm. The method described here can be applied to human serum, cell lysates, and low density lipoproteins.

티오바르비투릭 산 반응성 물질 분석체를 이용한 생물학적 시료의 산화 스트레스 평가

Despite its limited analytical specificity and ruggedness, the thiobarbituric acid reactive substances (TBARS) assay has been widely used as a generic ...