Gli autori vorrebbero riconoscere James A. Forrest aiuto per l&#39;idea iniziale di questa tecnica. 26 Questo lavoro è stato sostenuto da un finanziamento della University of Pennsylvania ed è stato parzialmente sostenuto dal programma MRSEC della National Science Foundation sotto premio n. DMR-11- 20901 presso l&#39;Università della Pennsylvania.

1. Film Preparazione <ol><li> Pesare 0,04 g di polistirene, e posto in una fiala da 30 ml. </li><li> Pesare 2 g di toluene nel flaconcino. A 2% in peso di soluzione di polistirene in toluene produce un film di circa 100 nm. </li><li> Lasciate che la soluzione di sit O / N per sciogliere completamente il polistirolo e lasciare che le soluzioni si depositano. </li><li> Posizionare un 1 cm x 1 cm silicio (Si) su un wafer di Coater Spin. </li><li> Gira la cialda a 8000 rpm per 45 secondi. Mentre gira, goccia circa 1 ml di toluene sul wafer filatura. Nota: Tutti i passi che coinvolgono spin coating vengono eseguiti in una cappa aspirante. </li><li> Sulla ora stazionaria Si wafer, aggiungere la soluzione proveniente dal passaggio 1,3 goccia a goccia sul wafer di Si finché l&#39;intera superficie del wafer di Si è coperto. </li><li> Prima soluzione asciuga sul wafer, centrifugare Si wafer a 4.000 rpm per 20 sec. </li><li> Determinare lo spessore della pellicola utilizzando ellissometria (vedere fase 2). </li><li> Se la pellicola è lo spessore desiderato, Anneal il film in stufa da vuoto a 393 K per 15 h. </li></ol> 2. Determinazione dello spessore del film <ol><li> Collocare la pellicola lanciare filata sul palco ellissometro e misurano gli angoli ellissometriche Ψ (λ) e Δ (λ) ad un angolo di luce incidente di 70 ° con un tempo di acquisizione 1 sec e l&#39;impostazione del fuso media accesi. </li><li> Utilizzando il software ellissometro, montare il Ψ risultante (λ) ei dati Δ (λ) per un modello a tre livelli secondo il protocollo del produttore. Non ci sono input dell&#39;utente aggiuntive. Il primo strato è uno strato di substrato di Si, il secondo strato è uno strato di ossido nativo con uno spessore di 1,5 nm, e il terzo strato è un modello Cauchy (n = A + B / λ 2, k = 0), il che corrisponde alle proprietà ottiche del film di polistirene. In questo modello, A e B sono parametri adatti, e n e k sono le componenti reale e immaginaria dell&#39;indice di rifrazione, rispettivamente. </li><li> Per lo strato di Cauchy, montare il thickness e parametri A e B, se il film è superiore a 10 nm. Se il film è inferiore a 10 nm, solo adattarsi A. Nota: Questo sarà discusso ulteriormente nella sezione risultati rappresentativi. </li></ol> 3. Raffreddamento Tasso Dipendente T g Misure <ol><li> Ricoprire la superficie dell&#39;elemento di riscaldamento della fase ellissometro temperatura variabile con pasta termica. </li><li> Posizionare il film di polistirene ricotto sull&#39;elemento riscaldante. </li><li> Fissare la pellicola saldamente l&#39;elemento riscaldante. </li><li> Flusso 100% gas azoto secco attraverso lo stadio di temperatura ad una pressione di &lt;69 KPa. </li><li> Utilizzando il software stadio di temperatura, creare un profilo di temperatura. Questo profilo di temperatura comincia con una rampa di riscaldamento di 393 K a 150 K / min. Tenere la pellicola per 393K per 20 min. <ol><li> Poi, le rampe di raffreddamento supplenti 293 K a tassi di 150, 120, 90, 60, 30, 10, 7, 3, e 1 K / min con rampe di riscaldamento a 393 K a 150 K / min. Posizionare un 5 min tempetura attesa dopo ogni rampa. </li></ol></li><li> Nel software ellissometro, fare un modello ellissometria dipendente temperatura simile a quella nella sezione 2. I tre strati sono identici, tranne per il substrato è cambiato ad una temperatura dipendente modello SI. </li><li> Nello strato per la temperatura in base al modello di Si, attivare il &quot;Usa Ext Temp da Parm registro&quot; Parametro. </li><li> Utilizzando attrezzature di laboratorio software di controllo, hanno il software ellissometro leggere i valori di temperatura da palcoscenico temperatura. </li><li> Allineare il ellipsometer tale che il segnale raggiunge la massima intensità. </li><li> Sotto &quot;Configurazioni Modifica hardware&quot;, impostare il tempo di acquisizione veloce di 1 sec con alta accuratezza zona media. Impostare il normale tempo di acquisizione di 3 sec con alta accuratezza zona media. </li><li> Nella scheda &quot;in situ&quot; nel software ellissometro controllare la &quot;modalità di acquisizione veloce tempo&quot; scatola, e premere &quot;Start Acquisition&quot;. Quindi, avviareil profilo di temperatura. Prima della rampa / min raffreddamento 3 K, deselezionare la casella veloce tempo di acquisizione. </li></ol> 4. Determinazione dei valori di Tg <ol><li> Esportare la temperatura e profili di spessore nel software grafica e l&#39;analisi preferito, e separare i dati di temperatura e di spessore per tutti i 9 velocità di raffreddamento. </li><li> Per spiegare l&#39;effetto della zona media durante l&#39;acquisizione della temperatura, prendere ogni valore di temperatura, e media con il valore di temperatura che lo precede, tale che T = (T i + T i-1) / 2, dove T i è un valore di temperatura in un dato momento, e T i-1 è la temperatura del punto di tempo precedente. </li><li> Trama Spessore vs. temperatura per ogni velocità di raffreddamento. </li><li> Eseguire una misura lineare su una porzione del regime Liquid Super raffreddato (regime alta temperatura con il coefficiente di espansione più grande). Tale regime sarà di circa da 393 K a 380 K. </li><li> Perform un&#39;interpolazione lineare su una porzione del regime vetrosa dello stesso insieme di dati. Questo regime ha un coefficiente di espansione inferiore, e sarà approssimativamente da 293 a 340 K K. </li><li> Trovare il punto di intersezione di queste due linee. La temperatura alla quale queste linee si intersecano è la temperatura di transizione vetrosa. </li><li> Fate questo per tutti i nove rampe. </li></ol> 5. Analisi media a pellicola sottile Dynamics <ol><li> Per un dato appezzamento spessore del film Log (Tasso di raffreddamento (K / min)) vs. 1 / T g (K -1). </li><li> Confronta questo indirettamente alle misurazioni dirette delle dinamiche di massa e di superficie dalla relazione empirica: Tasso di raffreddamento * τ α = 1000. 23,24 </li></ol>

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The Authors have no conflicts of interest to disclose.

Raffreddamento-velocità dipendente T g misurazioni sono high throughput esperimenti di caratterizzazione che possono determinare la g T, il coefficiente di dilatazione del vetro e il liquido super-raffreddato, la dipendenza dalla temperatura della dinamica media e la fragilità di un particolare materiale vetroso in un singolo esperimento. Inoltre, a differenza di fluorescenza, incorporamento o nanohole esperimenti di rilassamento, CR-T g esperimenti sono relativamente rapido e semplice...

Il lavoro seminale di Keddie Jones e Corey 1 ha mostrato che la temperatura di transizione vetrosa (Tg) di film di polistirene ultrasottili diminuisce rispetto al valore massa a spessori inferiori a 60 nm. Da allora, numerosi studi sperimentali 2-11 hanno sostenuto l&#39;ipotesi che le riduzioni osservate in T g sono causate da uno strato di una maggiore mobilità in prossimità della superficie libera di questi film. Tuttavia, questi esperimenti sono misure indirette di un unico tempo di rilassamento, e quindi non vi è un dibattito 12- 18 centrata su una correlazione diretta tra la media dinamica a film sottile e le dinamiche all&#39;interfaccia aria / polimero. Per rispondere a questo dibattito, molti studi hanno misurato direttamente la dinamica della superficie libera (superficie τ). Nanoparticelle incorporamento, 19,20 nanohole rilassamento, 21 e fluorescenza 22 studi dimostrano che l&#39;interfaccia aria / polimero hcome dinamica ordini di grandezza più veloce del tempo di rilassamento alfa massa (τ α) con una dipendenza dalla temperatura molto più debole di quella di τ α. A causa della sua debole dipendenza dalla temperatura, la superficie τ di questi film, 19-22 e migliorate dinamiche di film sottili di polistirene, 23,24 interseca il rilassamento alfa bulk (τ α) in un unico punto T *, che è a pochi gradi sopra T g, e ad un α τ di ≈ 1 sec. La presenza di T * potrebbe spiegare perché gli esperimenti che sondano tempi di rilassamento più veloce di * non riescono a vedere ogni dipendenza spessore sul g T di film in polistirene ultrasottili. 13-18 Infine, mentre le misurazioni dirette della maggiore manifestazione strato cellulare che ha uno spessore di 4-8 nm, 20-22 vi è evidenza che la lunghezza di propagazione delle dinamiche all&#39;interfaccia aria / polimero è molto più grande rispetto allo spessore del piano mobile layer. 5,25,26 La presente relazione mira a descrivere completamente un protocollo per l&#39;utilizzo di ellissometria per tasso dipendente T g (CR-T g) esperimenti di raffreddamento. CR-T g è stato precedentemente utilizzato per descrivere la dinamica medi di film ultrasottili di polistirene. 23,24,27,28 Inoltre, questa tecnica è stata recentemente utilizzata per mostrare una correlazione diretta tra la dinamica medi in film di polistirene ultrasottili , e le dinamiche sulla superficie libera. 23 Il vantaggio di CR-T g misurazioni rispetto ad altri tipi di misurazioni come la fluorescenza, nanoparticelle incorporamento, nanohole rilassamento, nanocalorimetry, spettroscopia dielettrica e light scattering Brillouin, studi è che sono relativamente veloce e semplici esperimenti che non utilizzano fluorofori o altre tecniche sperimentali complicate. I recenti progressi nella ellissometria spettroscopica consentono questa tecnica per essere utilizzato per determinare l&#39;efficienza ottica propertzioni del film ultrasottili di polimeri e di altri tipi di materiali ibridi con una precisione eccezionale. Come tale, questa tecnica sonda le dinamiche medi di film sottili tecnologicamente applicabili nei regimi di temperatura e di tempo relativi alla transizione vetrosa (T ≤ T g, τ α ≥ 100 sec). Inoltre, questa tecnica fornirà informazioni sui coefficienti di espansione del vitreo e cena raffreddato stati liquido e la fragilità del sistema, che può essere confrontato con i dati per film bulk. Infine, CR- T g esperimenti possono essere utilizzati per qualsiasi sistema vetroso fintanto che l&#39;integrità del film rimane tutto l&#39;esperimento.

<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

La presente relazione mira a descrivere pienamente la tecnica sperimentale di utilizzare ellissometria per tasso dipendente T g (CR-T g) esperimenti di raffreddamento. Queste misure sono semplici esperimenti di caratterizzazione di alto-rendimento, che possono determinare la temperatura di transizione vetrosa (T g), la dinamica media, fragilità e il coefficiente di dilatazione degli stati liquido e vetrosi super raffreddato per una varietà di materiali vetrosi. Questa tecnica permette di questi parametri da misurare in un singolo esperimento, mentre altri metodi devono combinare una varietà di tecniche diverse per indagare tutte queste proprietà. Misure di dinamica vicino ai Tg sono particolarmente impegnativi. Il vantaggio di raffreddamento dei tassi dipende Tg misure rispetto ad altri metodi che sondano direttamente le dinamiche di massa e di rilassamento superficie è che essi sono esperimenti relativamente semplici e veloci, che non utilizzano fluorofori o altri ex complicatotecniche sperimentali. Inoltre, questa tecnica sonda le dinamiche medi di film sottili tecnologicamente rilevanti di temperatura e tempo di rilassamento (τ α) regimi pertinenti alla transizione vetrosa (τ α&gt; 100 sec). La limitazione all&#39;utilizzo ellissometria per velocità di raffreddamento dipende T g esperimenti è che non può sondare tempi di rilassamento rilevanti per misurazioni di viscosità (τ α &lt;&lt; 1 sec). Altre velocità di raffreddamento dipende T tecniche di misura g, tuttavia, possono estendere il metodo CR-T g per tempi di rilassamento veloce. Inoltre, questa tecnica può essere utilizzata per qualsiasi sistema vetroso fintanto che l&#39;integrità del film rimane tutto l&#39;esperimento.

Raccordo grezzo ellissometria dati Film polistirolo sono trasparenti nella gamma di lunghezze d&#39;onda della ellissometro (500-1,600 nm). Così un modello Cauchy è un buon modello per descrivere l&#39;indice di rifrazione del film di polistirene. La figura 1A mostra un esempio di Ψ (λ) e Δ (λ) per una spessa (274 nm) pellicole di polistirene, e la misura ottenuta al modello di Cauchy <i...

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

Qui, presentiamo un protocollo per velocità di raffreddamento esperimenti dipendenti ellissometria, che possono determinare la temperatura di transizione vetrosa (Tg), dinamica media, fragilità e il coefficiente di dilatazione del liquido super-raffreddato e vetro per una varietà di materiali vetrosi.

Raffreddamento Vota dipendenti Misure ellissometria per determinare la dinamica dei Thin Films Glassy

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

cooling-rate-dependent-ellipsometry-measurements-to-determine

Research

JoVE Journal

Chemistry

8.1K Views.  University of Pennsylvania.  Qui, presentiamo un protocollo per velocità di raffreddamento esperimenti dipendenti ellissometria, che possono determinare la temperatura di transizione vetrosa (Tg), dinamica media, fragilità e il coefficiente di dilatazione del liquido super-raffreddato e vetro per una varietà di materiali vetrosi. 

Video: 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.

Strato sottile cromatografica (TLC) Separazioni e Bioassays di estratti vegetali per identificare composti antimicrobici

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

Ricerca

Chimica

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.

Modelli atomicamente definiti per epitassiale crescita di ossido Complex Thin Films

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.

Alte le misure di precisione di zinco isotopiche applicate a mouse Organi

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.

Fabbricazione di ampia superficie Free-standing ultrasottili film polimerici

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.

Svelare entropico velocità di accelerazione indotta da solventi Dynamics a membrana Enzimi

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.

Scioglimento dinamica nucleare Polarizzazione Strumentazione in tempo reale enzimatica di reazione misure di frequenza di risonanza magnetica nucleare

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.

Elettroforesi capillare per monitorare Peptide innesto su Chitosano film in tempo reale

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.

Spettroscopia di impedenza elettrochimica come uno strumento per la stima della costante tasso elettrochimica

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.

Deposizione di vapore reattiva di film polimerici coniugati su substrati arbitrari

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.

Soluzione di elaborazione "Silver-bismuto-iodio" ternario pellicole sottili per assorbitori di piombo fotovoltaici

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