저자는이 기술에 대한 초기 아이디어에 도움을 제임스 포레스트을 인정하고 싶습니다. (26)이 작품은 펜실베니아 대학에서 기금에 의해 지원되었다 부분적으로없는 상 아래에있는 국립 과학 재단 (National Science Foundation)의 MRSEC 프로그램에 의해 지원되었다. DMR-11- 펜실베니아 대학에서 20,901.

1. 영화 준비 <ol><li> 폴리스티렌의 0.04 g의 무게를 측정하고, 30 ㎖의 유리 병에 넣습니다. </li><li> 유리 병에 톨루엔 2g의 무게. 톨루엔 폴리스티렌 용액의 중량에 의해 2 %은 약 100 nm의 피막을 산출한다. </li><li> 솔루션 앉아 O / N 완전히 폴리스티렌을 용해 및 솔루션 정착 있도록하자. </li><li> 스핀 코터에 1cm X 1cm의 실리콘 (Si) 웨이퍼를 놓습니다. </li><li> 45 초 동안 8000 rpm에서 스핀 웨이퍼. 이 구동 중일 때, 회전하는 웨이퍼 상에 톨루엔 약 1ml를 놓는다. 주 : 스핀 코팅을 포함한 모든 단계 흄 후드에서 수행된다. </li><li> Si 웨이퍼의 전체 표면이 피복되어 지금까지 고정 Si 웨이퍼 상에, Si 웨이퍼 상에 1.3 적가 단계에서 용액을 추가한다. </li><li> 용액을 웨이퍼 상에 건조하기 전에 20 초 동안 4000 rpm에서 Si 웨이퍼를 스핀. </li><li> 엘립 소메 트리를 사용하여 필름의 두께를 결정한다 (단계 2 참조). </li><li> 필름은 원하는 두께, 앤이면15 시간 동안 393 K에서의 진공 오븐에서 필름 EAL. </li></ol> 2. 도막 두께를 결정 <ol><li> 타원의 무대에 스핀 캐스트 필름을 놓고 1 초 획득 시간과 영역 평균 설정으로 70 °의 입사 각도에서 엘 립소 각도 Ψ (λ)와 Δ (λ) 켜져 측정한다. </li><li> 엘 립소 소프트웨어를 사용하여 제조사의 프로토콜에 따른 3 층 모델 생성 Ψ (λ)과 Δ (λ)의 데이터를 장착한다. 추가 사용자 입력이 없습니다. 제 1 층의 Si 기판 층이고, (N = A는 B / λ 2, K = 0 +), 이는 대응하는 제 2 층은 1.5 nm 두께의 자연 산화물 층이고, 제 3 층은 코시 모델 폴리스티렌 필름의 광학 특성에 관한 것이다. 이 모델에서, 그리고 B는 적합 파라미터이고, n 및 k는 각각의 굴절률의 실수 및 허수 성분이다. </li><li> 코시 층, t 맞게hickness 및 파라미터와 B가 10 nm의 막보다 큰 경우. 막은 10 내지 이하인 경우에만 맞. 주 :이 대표 결과 섹션에서 더 논의 될 것이다. </li></ol> 3. 냉각 속도 종속 Tg를 측정 <ol><li> 코트 열 페이스트 가변 온도 립소 단의 발열체의 표면. </li><li> 가열 요소에 어닐링 폴리스티렌 필름을 놓습니다. </li><li> 발열체 상에 단단히 필름 클램프. </li><li> &lt;69 인민군 압력에서 온도 단계를 통해 100 % 건조 질소 가스가 흐르. </li><li> 온도 스테이지 소프트웨어를 사용하여 온도 분포를 만든다. 이 온도 프로파일은 150 K / 분으로 393 K까지 가열 램프로 시작된다. 20 분 동안 393K에서 영화를 잡습니다. <ol><li> 그런 다음의 가격을 293 K까지 냉각 대체 램프 150, 120, 90, 60, 30, 10, 7, 150 K / 분으로 393 K까지 가열 램프와 3 및 1 K / 분. 5 분 템피 배치각각의 램프 후 rature 유지. </li></ol></li><li> 엘 립소 소프트웨어에서, 기판은 온도 의존 실리콘 모델로 변경하는 것을 제외하고 모든 세 개의 층이, 동일한 제 2 항에서와 온도 의존 엘립 소메 트리 모델은 유사하게. </li><li> 온도 의존시 모델의 레이어에서 매개 변수 &quot;PARM 로그에서 사용 내선 온도&quot;를 켭니다. </li><li> 실험 장비 제어 소프트웨어를 사용하여, 엘 립소 소프트웨어 온도 단계에서 온도 값을 읽게한다. </li><li> 신호가 최대 강도에 도달하도록 타원을 맞 춥니 다. </li><li> &quot;편집 하드웨어 구성&quot;에서 고정밀 영역 평균 1 초에 빠른 취득 시간을 설정합니다. 고정밀 영역 평균 3 초에 정상 획득 시간을 설정합니다. </li><li> 타원 소프트웨어에서 &quot;현장에서&quot;탭에서 &quot;빠른 획득 시간 모드&quot;상자를 누릅니다 &quot;시작 취득&quot;을 선택합니다. 그런 다음, 시작온도 프로파일. 3 K / min의 냉각 램프 전에 빠른 획득 시간의 선택을 취소합니다. </li></ol> 4. T (G)의 값을 결정 <ol><li> 선호하는 그래프 및 분석 소프트웨어에 온도와 두께 프로파일을 내 보낸 모든 9 냉각 속도에 대한 온도 및 두께 데이터를 구분합니다. </li><li> 온도에 취득시 영역 평균화의 효과를 설명마다 온도 값을, 그리고 T는 = / 2, 여기서 T의 I (T 난 -1- T를 +)되도록, 그 앞에 온도 값과 평균 위해서는 온도 주어진 시간 값, 그리고 T는 I-1은 선행하는 시점의 온도이다. </li><li> 각각의 냉각 속도에 대한 온도 대 플롯 두께. </li><li> 슈퍼 냉각 액체 체제 부분에 선형 피팅 (큰 팽창 계수 고온 체제)을 수행한다. 이 정권은 393 K에서 380 K를 약 것입니다 </li><li> PERFO동일한 데이터 세트의 유리 정권의 일부에 선형 피팅 RM. 이 체계는 낮은 열팽창 계수를 가지며, 293 K에서 약 340 K. 것 </li><li> 이들 두 라인의 교차점을 찾을. 이들 라인이 교차하는 온도를 유리 전이 온도이다. </li><li> 모든 구 램프에 대해이 작업을 수행합니다. </li></ol> 5. 평균 박막 역학 분석 <ol><li> 주어진 필름 두께 플롯 로그 (냉각 속도 (K / 분)) 대 1 / T의 G (K-1)의 경우. </li><li> 경험적인 관계에 의해 벌크 및 표면 역학의 측정을 직접 간접적으로 비교 : 냉각 속도 * τ α = 1000 (23, 24) </li></ol>

<ol>
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D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Confined+glassy+properties+of+polymer+nanoparticles.">Confined glassy properties of polymer nanoparticles.</a> J. Polym. Sci. B. 51 (7), 574-586 (2013).</li><li>Koh, Y. P., Grassia, L., Simon, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+Recovery+of+a+Single+Polystyrene+Thin+Film+Using+Nanocalorimetry+to+Extend+the+Aging+Time+and+Temperature+Range.">Structural Recovery of a Single Polystyrene Thin Film Using Nanocalorimetry to Extend the Aging Time and Temperature Range.</a> Thermochimica Acta. 603, 135-141 (2015).</li><li>Gao, S., Simon, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Measurement+of+the+limiting+fictive+temperature+over+five+decades+of+cooling+and+heating+rates.">Measurement of the limiting fictive temperature over five decades of cooling and heating rates.</a> Thermochimica Acta. 603, 123-127 (2015).</li></ol>

The Authors have no conflicts of interest to disclose.

냉각 속도 의존성의 Tg 측정은 T의 g, 유리 및 과냉각 액체, 평균 역학의 온도 의존성의 팽창 계수와의 특정 유리질 재료의 취약성을 판별 할 수있는 높은 작업 처리량 특성화 실험 아르 하나의 실험. 그들은 형광 또는 다른 복잡한 실험 기법을 활용하지 않기 때문에 또한, 형광, 매립 또는 나노 홀 완화 실험 달리 CR-T g의 실험은 비교적 빠르고 간단하다. 엘립 소메 의한 감도...

Keddie 존스 코리 1 정액 일 초박형 폴리스티렌 필름의 유리 전이 온도 (T g)을 60 nm의 두께에서보다 낮은 벌크 값에 대해 감소한다는 것을 보여 주었다. 그 이후, 많은 연구 실험 2-11의 T g에서 관찰 된 감소는 이러한 막의 자유 표면 근처에 의해 향상된 이동도의 층에 의해 야기되는 가설을지지하고있다. 그러나,이 실험은 단일 완화 시간의 간접 측정이 있고, 따라서 평균 박막 역학 및 공기 / 폴리머 계면에서 역학 사이에 직접적인 상관 관계를 중심으로 논의 12- 18있다. 이 논쟁에 대답하기 위해, 많은 연구는 직접 자유 표면 (τ면)의 역학을 측정했다. 나노 입자 삽입, 19, 20 나노 홀 휴식, 21, 형광 22 연구는 보여 그 공기 / 폴리머 인터페이스 H빠른 τ의 α보다 훨씬 약한 온도 의존성을 가진 벌크 알파 완화 시간 (τ α)보다 크기의 차수로서 역학. 때문에 그 약한 온도 의존성,이 영화의 τ의 표면은 얇은 폴리스티렌 필름의 19 ~ 22 향상된 역학, 23, 24 위 몇도 단일 포인트 T의 *에서 (τ α) 대량 알파 휴식을 교차 T는 g 및 ≈ 1 초 τ (α)에서. 빠른 * 이상의 휴식 시간을 조사 실험 초박형 폴리스티렌 필름의 T g로 모든 두께 의존성을보고 실패 이유 T의 *의 존재를 설명 할 수있다. 13 ~ 18 마지막으로, 동안이 가지고있는 향상된 모바일 계층 쇼의 직접 측정 4-8 nm의 두께는, 20 ~ 22은 공기 / 폴리머 계면에서 역학의 전파 길이 모바일 Laye의 표면의 두께보다 훨씬 크다는 것을 증거가R. 5,25,26 이보고는 완전 레이트 종속 된 T g (CR-T의 g) 실험을 냉각하기위한 엘립 소메 트리를 이용하기위한 프로토콜을 기술하는 것이다. CR-T g는 이전의 폴리스티렌의 초박막의 평균 역학을 설명하는 데 사용되어왔다. 23,24,27,28 또한,이 기술은 최근에 사용 된 초박형 폴리스티렌 필름의 역학 평균 사이의 직접적인 상관 관계를 보여 자유 표면에서, 및 역학. (23)와 같은 형광 나노 입자 매립, 나노 홀 이완 nanocalorimetry 유전체 분광법 및 브릴 루앙 광 산란과 같은 다른 유형의 측정을 통해 CR-T의 g 측정의 장점은, 연구들은 비교적 빠른 점이다 간단한 실험은 형광 또는 다른 복잡한 실험 기술을 사용하지 않는. 분광 엘립 소메 최근 발전은이 기술을 효율적으로 광 PROPERT를 결정하는데 이용 될 수 있도록중합체 및 뛰어난 정밀도 하이브리드 재료의 다른 형태의 초박막의 IES. 이와 같이,이 기술은 유리 전이 (T ≤ T의 g, τ α ≥ 100 초)에 관련된 온도 및 시간 정권 기술적 적용 박막의 평균 동역학을 프로빙. 또한,이 기술은 유리의 팽창 계수에 대한 정보를 제공하며 만찬 액체 상태뿐만 아니라 후 벌크 필름 데이터와 비교 될 수있는 시스템의 취약성을 냉각시켰다. 마지막으로, T CR- g의 실험은 너무 긴 필름의 무결성이 실험 전반에 걸쳐 유지되는 임의의 유리 시스템에 사용될 수있다.

<table border="0" cellpadding="0" cellspacing="0" width="918">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Toluene</td>
			<td style="width:111px;">Sigma Aldrich</td>
			<td style="width:119px;">179418-1L</td>
			<td style="width:472px;">This can be purchased from any chemical company.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Atactic Polystyrene</td>
			<td style="width:111px;">Polymer Source Inc.</td>
			<td style="width:119px;">P-4092-S</td>
			<td>This can be purchased from any chemical company.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">THMS 600 temperature stage</td>
			<td style="width:111px;">Linkam</td>
			<td style="width:119px;">THMS 600</td>
			<td>any temperature stage that can be fit to an ellipsometer could be used.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">M2000V Spectroscopic Ellipsometer</td>
			<td style="width:111px;">J.A. Woollam</td>
			<td style="width:119px;">M200V</td>
			<td>This procedure should be applicable for any spectroscopic ellipsometer.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Spin Coater</td>
			<td style="width:111px;">Laurell Technologies</td>
			<td style="width:119px;">WS-650-23B</td>
			<td>This Procedure is possible with any spin coater</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Sample vials</td>
			<td style="width:111px;">Fisher Scientific</td>
			<td style="width:119px;">02-912-379</td>
			<td>Any sample vials will do</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Silicon wafers</td>
			<td style="width:111px;">Virginia semi conductors</td>
			<td style="width:119px;">325S1410694D</td>
			<td></td>
		</tr>
	</tbody>
</table>

cooling rate dependent ellipsometry measurements to determine the dynamics of thin glassy films

이보고는 완전 레이트 종속 된 T g (CR-T의 g) 실험을 냉각하기위한 엘립 소메 트리를 사용하는 실험 방법을 설명하는 것이다. 이러한 측정은 유리 전이 온도를 결정할 수있는 간단한 높은 처리량 특성화 실험 아르 (T의 g), 평균 동역학, 취약성 및 유리질 재료의 다양한 과냉각 액체 및 유리 상태의 팽창 계수. 이 기술은 다른 방법이 이러한 모든 특성을 조사하기 위해 서로 다른 다양한 기술을 결합해야하는 동안 이러한 파라미터는, 하나의 실험에서 측정 할 수 있습니다. 역학의 측정은 T의 G에 가까운 특히 도전이다. 직접 벌크 및 표면 완화 역학 프로브 다른 방법에 비해 속도 의존성의 T g 측정 냉각 장점은 형광 또는 다른 복잡한 예를 이용하지 않은 비교적 빠르고 간단한 실험 때문이다perimental 기술. 또한,이 기술은 유리 전이 (τ (α)&gt; 100 초)에 관련된 온도와 휴식 시간에 과학 기술 관련 박막 (τ α) 정권의 평균 역학을 조사합니다. 속도 의존 T g의 실험을 냉각하기위한 엘립 소메 트리를 사용하는 제한 (τ α &lt;&lt; 1 초)의 점도가 측정을 완화 시간이 중요한 조사 할 수 없다는 것이다. 다른 냉각 속도 의존성 T g 측정 기술은, 그러나 빠르게 완화 시간에 CR-T g의 방법을 확장 할 수있다. 또한,이 기술은 매우 긴 필름의 무결성이 실험 전반에 걸쳐 유지되는 임의의 유리 시스템에 사용될 수있다.

피팅 원시 일립 소미 트리는 데이터 폴리스티렌 필름은 타원 (500-1,600 ㎚)의 파장 범위에서 투명하다. 따라서 코시 모델 폴리스티렌 필름의 굴절률을 설명하기위한 좋은 모델이다.도 1a는 폴리스티렌의 두께 (274 ㎚) 필름, 그리고 그 결과 얻어지는 착용감 Ψ (λ)과 Δ (λ)의 예를 나타낸다 코시 모델 <img a...

Watch this Scientific Journal Video about Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films at JoVE.com

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

여기서는 유리 재료의 다양한 속도 유리 전이 온도 (T g)을 결정할 수 종속 엘립 소메 실험, 평균 동역학, 취약성 및 과냉각 액체의 팽창 계수와 유리를 냉각하기위한 프로토콜을 제시한다.

속도 종속 엘립 소메 트리 측정 냉각 얇은 유리 필름의 역학을 확인하는

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

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Chemistry

8.1K 조회수.  University of Pennsylvania.  여기서는 유리 재료의 다양한 속도 유리 전이 온도 (T g)을 결정할 수 종속 엘립 소메 실험, 평균 동역학, 취약성 및 과냉각 액체의 팽창 계수와 유리를 냉각하기위한 프로토콜을 제시한다. 

비디오: Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

Thin-layer Chromatographic (TLC) Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth.&#160;The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken with microbial culture conditions.&#160;This paper describes standard protocols for TLC and contact bioautography&#160;with a novel application to amino acid-fermenting bacteria. The extract is separated on flexible (aluminum-backed) silica TLC plates, and bands are visualized under ultraviolet (UV) light.&#160;Zones are cut out and incubated face down onto agar inoculated with the test microorganism.&#160;Inhibitory bands are visualized by staining the agar plates with tetrazolium red.&#160;The method is applied to the separation of red clover (Trifolium pratense cv. Kenland) phenolic compounds and their screening for activity against Clostridium sticklandii, a hyper ammonia-producing bacterium (HAB) that is native to the bovine rumen.&#160;The TLC methods apply to many types of plant extracts&#160;and other bacterial species (aerobic or anaerobic), as well as fungi, can be used as test organisms if culture conditions are modified to fit the growth requirements of the species.

Thin-layer Chromatographic TLC Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

Methods are described for thin-layer chromatographic (TLC) separation of plant extracts and contact bioautography to identify antibacterial metabolites. The methods are applied to the screening of red clover phenolic compounds inhibiting hyper&#160;ammonia-producing bacteria (HAB) native to the bovine rumen.

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the ...

연구

화학

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

복합 산화물 박막의 에피 택셜 성장을위한 원자 적으로 정의 된 템플릿

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

High Precision Zinc Isotopic Measurements Applied to Mouse Organs

We present a procedure to measure with high precision zinc isotope ratios in mouse organs. Zinc is composed of 5 stable isotopes (64Zn, 66Zn, 67Zn, 68Zn and 70Zn) which are naturally fractionated between mouse organs. We first show how to dissolve the different organs in order to free the Zn atoms; this step is realized by a mixture of HNO3 and H2O2. We then purify the zinc atoms from all the other elements, in particular from isobaric interferences (e.g., Ni), by anion-exchange chromatography in a dilute HBr/HNO3 medium. These first two steps are performed in a clean laboratory using high purity chemicals. Finally, the isotope ratios are measured by using a multi-collector inductively-coupled-plasma mass-spectrometer, in low resolution. The samples are injected using a spray chamber and the isotopic fractionation induced by the mass-spectrometer is corrected by comparing the ratio of the samples to the ratio of a standard (standard bracketing technique).&#160;This full typical&#160;procedure produces an isotope ratio with a 50 ppm (2 s.d.) reproducibility.

We present the technique to measure with high precision zinc isotope ratios in mouse organs.

마우스 기관에 적용 높은 정밀도 아연 동위 원소 측정

We present a procedure to measure with high precision zinc isotope ratios in mouse organs. Zinc is composed of 5 stable isotopes (64Zn, 66Zn, 67Zn, 68Zn ...

Fabrication of Large-area Free-standing Ultrathin Polymer Films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

대 면적의 제작은 초박막 고분자 필름을 무료 서

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

Unraveling Entropic Rate Acceleration Induced by Solvent Dynamics in Membrane Enzymes

Enzyme catalysis evolved in an aqueous environment. The influence of solvent dynamics on catalysis is, however, currently poorly understood and usually neglected. The study of water dynamics in enzymes and the associated thermodynamical consequences is highly complex and has involved computer simulations, nuclear magnetic resonance (NMR) experiments, and calorimetry. Water tunnels that connect the active site with the surrounding solvent are key to solvent displacement and dynamics. The protocol herein allows for the engineering of these motifs for water transport, which affects specificity, activity and thermodynamics. By providing a biophysical framework founded on theory and experiments, the method presented herein can be used by researchers without previous expertise in computer modeling or biophysical chemistry. The method will advance our understanding of enzyme catalysis on the molecular level by measuring the enthalpic and entropic changes associated with catalysis by enzyme variants with obstructed water tunnels. The protocol can be used for the study of membrane-bound enzymes and other complex systems. This will enhance our understanding of the importance of solvent reorganization in catalysis as well as provide new catalytic strategies in protein design and engineering.

Channels for the transportation of water molecules in enzymes influence active site solvation and catalysis. Herein we present a protocol for the engineering of these additional catalytic motifs based on in silico computer modeling and experiments. This will enhance our understanding of the influence of solvent dynamics on enzyme catalysis.

막 효소 용매 역학에 의해 유도 탈피 엔트 속도 가속

Enzyme catalysis evolved in an aqueous environment. The influence of solvent dynamics on catalysis is, however, currently poorly understood and usually ...

Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

The main limitation of NMR-based investigations is low sensitivity. This prompts for long acquisition times, thus preventing real-time NMR measurements of metabolic transformations. Hyperpolarization via dissolution DNP circumvents part of the sensitivity issues thanks to the large out-of-equilibrium nuclear magnetization stemming from the electron-to-nucleus spin polarization transfer. The high NMR signal obtained can be used to monitor chemical reactions in real time. The downside of hyperpolarized NMR resides in the limited time window available for signal acquisition, which is usually on the order of the nuclear spin longitudinal relaxation time constant, T1, or, in favorable cases, on the order of the relaxation time constant associated with the singlet-state of coupled nuclei, TLLS. Cellular uptake of endogenous molecules and metabolic rates can provide essential information on tumor development and drug response. Numerous previous hyperpolarized NMR studies have demonstrated the relevancy of pyruvate as a metabolic substrate for monitoring enzymatic activity in vivo. This work provides a detailed description of the experimental setup and methods required for the study of enzymatic reactions, in particular the pyruvate-to-lactate conversion rate in presence of lactate dehydrogenase (LDH), by hyperpolarized NMR.

The sensitivity enhancement provided by dissolution dynamic nuclear polarization (DNP) enables following metabolic processes in real time by NMR and MRI. The characteristics and performances of a dedicated dissolution DNP setup designed for study enzymatic reactions are discussed.

The main limitation of NMR-based investigations is low sensitivity. This prompts for long acquisition times, thus preventing real-time NMR measurements of ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. Compared to other analytical separation techniques, such as chromatography, CE is cheap, robust and effectively requires no sample preparation (for a number of complex natural matrices or polymeric samples). CE is fast and can be used to follow the evolution of mixtures in real time (e.g., chemical reaction kinetics), as the signals observed for the separated compounds are directly proportional to their quantity in solution.
Here, the efficiency of CE is demonstrated for monitoring the covalent grafting of peptides onto chitosan films for subsequent biomedical applications. Chitosan&#39;s antimicrobial and biocompatible properties make it an attractive material for biomedical applications such as cell growth substrates. Covalently grafting the peptide RGDS (arginine - glycine - aspartic acid - serine) onto the surface of chitosan films aims at improving cell attachment. Historically, chromatography and amino acid analysis have been used to provide a direct measurement of the amount of grafted peptide. However, the fast separation and absence of sample preparation provided by CE enables equally accurate yet real-time monitoring of the peptide grafting process. CE is able to separate and quantify the different components of the reaction mixture: the (non-grafted) peptide and the chemical coupling agents. In this way the use of CE results in improved films for downstream applications.
The chitosan films were characterized through solid-state NMR (nuclear magnetic resonance) spectroscopy. This technique is more time-consuming and cannot be applied in real time, but yields a direct measurement of the peptide and thus validates the CE technique.

Free solution capillary electrophoresis is a fast, cheap and robust analytical method that enables the quantitative monitoring of chemical reactions in real time. Its utility for rapid, convenient and precise analysis is demonstrated here through analysis of covalent peptide grafting onto chitosan films for improved cell adhesion.

모세관 전기 영동은 실시간으로 키토산 필름에 펩타이드 접목을 모니터링하는

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

전기 화학 임피던스 분 광 전기 화학 속도 상수 추정을 위한 도구로

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

임의 기판에 활용 된 고분자 필름의 반응성 증 착

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. However, poor surface morphologies and relatively high bandgap energies have limited their potential. Silver-bismuth-iodine (Ag-Bi-I) is a promising semiconductor for optoelectronic devices. Therefore, we demonstrate the fabrication of Ag-Bi-I ternary thin films using material solution processing. The resulting thin films exhibit controlled surface morphologies and optical bandgaps according to their thermal annealing temperatures. In addition, it has been reported that Ag-Bi-I ternary systems crystallize to AgBi2I7, Ag2BiI5, etc. according to the ratio of the precursor chemicals. The solution-processed AgBi2I7 thin films exhibit a cubic-phase crystal structure, dense, pinhole-free surface morphologies with grains ranging in size from 200 to 800 nm, and an indirect bandgap of 1.87 eV. The resultant AgBi2I7 thin films show good air stability and energy band diagrams, as well as surface morphologies and optical bandgaps suitable for lead-free and air-stable single-junction solar cells. Very recently, a solar cell with 4.3% power conversion efficiency was obtained by optimizing the Ag-Bi-I crystal compositions and solar cell device architectures.

Herein, we present detailed protocols for solution-processed silver-bismuth-iodine (Ag-Bi-I) ternary semiconductor thin films fabricated on TiO2-coated transparent electrodes and their potential application as air-stable and lead-free optoelectronic devices.

솔루션 처리 "실버-비스무트-요오드" 삼항 박막 리드 무료 태양광 흡수에 대 한

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. ...