This work has been performed at the Molecular Foundry, Lawrence Berkeley National Laboratory and supported by the Office of Science, Office of Basic Energy Sciences, Scientific User Facilities Division of the US Department of Energy, under Contract No. DE-AC02&#8211;05CH11231. The financial support of F.M. by a ME-Fulbright fellowship and A.S. by Higher Education Commission of Pakistan are gratefully acknowledged.

NOTA: Prima di iniziare, controllare tutti i fogli competenti, dati materiali (MSDS). Molti dei prodotti chimici utilizzati nelle procedure di sintesi e di applicazione sono tossici. Si prega di seguire tutte le pratiche di sicurezza appropriate e utilizzare attrezzature adeguate di protezione (camice, pantaloni full-length, scarpe chiuse, occhiali di sicurezza, guanti). Si prega di utilizzare tutte le criogeniche dispositivi di protezione individuale durante la manipolazione di azoto liquido per le misure di adsorbimento di azoto (guanti isolanti, visiera). 1. poroso Polymer Monolith preparazione in massa e capillare Formatta colonna <ol><li> Bulk Polymer Monolith per la caratterizzazione <ol><li> Purificare stirene, divinilbenzene e acido metacrilico attraverso una colonna di allumina basica, al fine di rimuovere gli inibitori di polimerizzazione. Introdurre 10 g di allumina basica in una siringa di plastica monouso ml 25 con un tappo in fibra di lana di vetro confezionato nella punta della siringa. Percolare circa 10 ml del monomero attraverso la colonna. </li><li> Caricare i monomeri (50 mg stirene, 100 mg divinilbenzene e 50 mg di acido metacrilico) e gli agenti che formano pori (300 mg toluene e 300 mg) in isoottano un flaconcino di vetro da 1 ml. Aggiungere l&#39;iniziatore della polimerizzazione, 4 mg di 2,2&#39;-azobisisobutirronitrile (AIBN, 1% rispetto ai monomeri). </li><li> Omogeneizzare mediante sonicazione per 10 min. Rimuovere l&#39;ossigeno dissolto con gorgogliamento di azoto attraverso il liquido per 10 min. Sigillare il cappuccio della fiala con parafilm e metterlo in un bagno di acqua a 60 ° C per 6 ore per polimerizzare la miscela. </li><li> Raffreddare a temperatura ambiente e rompere la fiala con attenzione. Trasferire il monolite di polimero in un ditale di estrazione della cellulosa. Porre il ditale di estrazione in una camera di estrazione Soxhlet e assemblare in un pallone a fondo tondo che contiene un volume di metanolo, che è almeno tre volte il volume della camera di estrazione. Assemblare un condensatore per la parte superiore della camera di estrazione. Eseguire l&#39;estrazione Soxhlet facendo bollire il metanoloper 16 ore, assicurando la completa rimozione dei monomeri non reagiti e poro agenti formatura. </li><li> Durante la notte a secco in un forno a vuoto a 60 ° C. Confermare la presenza di gruppi funzionali carbossilici per fissare la PCP Fourier Transform Infrared Spectroscopy (FT-IR). Misurare la superficie da adsorbimento di azoto porosimetria. </li></ol></li><li> Funzionalizzazione di silice capillari per la preparazione di colonne monolitiche <ol><li> Tagliare 2 m di 100 micron id capillare di silice fusa poliimmide rivestita. Collegare ad una siringa di vetro 0,25-0,50 ml e lavare il capillare con acetone. Rimuovere l&#39;acetone risciacquando capillare con acqua. </li><li> Per attivare il rivestimento di silice interna del capillare, utilizzare una pompa a siringa a fluire una soluzione di NaOH 0,2 M acquosa a 0,25 ml / min per 30 min. Risciacquare con acqua fino a quando l&#39;effluente è neutro. </li><li> Utilizzare strisce di carta pH per verificare dell&#39;effluente pH. Per protonare i gruppi silanolo del capillare, pompare un aqueo 0.2 Msoluzione ci HCl attraverso il capillare a 0.25 ml / min per 30 min. Risciacquare con acqua fino a quando l&#39;effluente è neutro. Sciacquare con etanolo. </li><li> Pompa a 20% (w / w) soluzione etanolica di 3- (trimetossisilil) propil metacrilato (pH 5 regolato con acido acetico) in 0,25 ml / min per 1 ora. In questa fase, il capillare di silice è funzionalizzato con gruppi vinilici per collegare il monolite polimero alla superficie interna capillare. </li><li> Risciacquare con acetone, secco in corrente di azoto e lasciare a temperatura ambiente per una notte prima dell&#39;uso. Tagliare il capillare in brevi pezzi di lunghezza 20 cm. </li></ol></li><li> Preparazione di colonne monolitiche capillari <ol><li> Preparare una miscela di polimerizzazione identico per il polimero monolite bulk (punto 1.1) in una fiala di vetro da 1 ml con un setto di gomma. Aggiungere iniziatore 1% AIBN rispetto ai monomeri. Omogeneizzare mediante sonicazione per 10 min. </li><li> Eliminare la miscela di polimerizzazione con azoto accoppiando un capillare di silice non-funzionalizzatoa un flusso di azoto. <ol><li> Inserire la corrente di azoto capillare attraverso il setto di gomma del flacone ed immergerlo nella miscela di polimerizzazione in modo che l&#39;azoto bolle nel liquido. Lasciare il tappo flacone leggermente allentato per evitare sovrapressione. Purge per 10 min. </li><li> Sollevare il capillare corrente di azoto dalla miscela di polimerizzazione allo spazio di testa della fiala, e chiudere ermeticamente il tappo. Inserire un capillare funzionalizzato attraverso il setto nella miscela di polimerizzazione. L&#39;eccesso di pressione generata nel capillare attraverso l&#39;azoto iniettato spazio di testa pompe miscela di polimerizzazione attraverso il capillare funzionalizzato. </li><li> Raccogliere alcune gocce di miscela di polimerizzazione dall&#39;effluente del capillare per assicurarsi che sia completamente riempito e chiuderlo con un setto di gomma. Prendere il capillare dal flaconcino con molta attenzione e chiudere l&#39;ingresso del capillare con un setto di gomma. </li></ol></li><li> Polimerizzare il mixture contenuta nel capillare in un bagno di acqua a 60 ° C per 6 ore. Raffreddare a temperatura ambiente e tagliare qualche millimetro di entrambe le estremità del capillare. Rimuovere monomeri non reagiti e agenti che formano pori svuotando la colonna con acetonitrile usando una pompa HPLC a 3 ml / min per 30 min. Controllare contropressione della colonna capillare. </li></ol></li></ol> 2. Crescita del ferro benzenetrycarboxylate (FeBTC) PCP <ol><li> La crescita della FeBTC MOPH su una massa Polymer Monolith per la caratterizzazione <ol><li> Macinare il monolite precedentemente essiccato con un mortaio e pestello. </li><li> Immergere 100 mg della polvere monolite in 5 ml di 2 mM FeCl 3 · 6H 2 O in etanolo per 15 min. Filtro a vuoto usando un filtro di nylon (0,22 micron) e lavare la polvere con etanolo. Immergere la polvere monolite in 5 ml di 2 mM di acido 1,3,5-benzenetricarboxylic (BTC) in etanolo per 15 min. Filtro a vuoto usando un filtro di nylon (0,22 micron) e lavare la polvere con etanolo.</li><li> Ripetere il passo numero 2 come desiderato. La crescita del rivestimento metallo-organico finale sarà definito dal numero di cicli richiesti. Tipicamente, vengono eseguiti tra 10 e 30 cicli. Confermare la presenza di nuovi pori mediante adsorbimento di azoto porosimetria. Misurare la quantità di siti di metallo supplementari di analisi termogravimetrica (TGA). </li></ol></li><li> La crescita della FeBTC MOPH su una colonna monolitica capillare per l&#39;arricchimento di fosfopeptidi <ol><li> Utilizzando una pompa a siringa. Lavare il monolite capillare con 2 mM FeCl 3 · 6H 2 O in etanolo per 15 minuti a 2 microlitri / min. Lavare con etanolo per 15 minuti a 2 microlitri / min. Lavare il monolito capillare con un BTC 2 mM in etanolo per 15 minuti a 2 microlitri / min. Lavare con etanolo per 15 minuti a 2 microlitri / min. </li><li> Ripetere il passaggio 1 come desiderato. La crescita del rivestimento metallo-organico finale sarà definito dal numero di cicli eseguiti. </li></ol></li></ol> 3. digestione delle proteine ​​ed Enrichment di fosfopeptidi <ol><li> Digestione delle proteine <ol><li> Sciogliere 0,5 ml di latte scremato in 1 ml di acqua e dividerlo in 200 microlitri frazioni. </li><li> Per la digestione delle proteine ​​aggiungere 160 microlitri 1 M di bicarbonato di ammonio e ditiotreitolo 50 microlitri 45 mM per ogni frazione, per aderire i legami disolfuro. Incubare a 50 ° C in un thermomixer per 15 min. </li><li> Aggiungere gradualmente 50 ml di una soluzione acquosa di iodoacetamide 100 mM, mentre la soluzione raffreddata a temperatura ambiente. Iodoacetamide impedirà la formazione di nuovi legami disolfuro. </li><li> Incubare al buio per 15 min a temperatura ambiente. Aggiungere 1 ml di acqua deionizzata. Aggiungere 2 ug tripsina e digerire le proteine ​​in un thermomixer a 37 ° C per 14 ore. </li><li> Terminare la digestione per acidificazione con 10 ml di 1% di acido trifluoroacetico, e ponendolo nella thermomixer per 5 min a temperatura ambiente. Conservare le proteine ​​digerite a -20 ° C. </li></ol></li><li> Arricchimento di fosfopeptidi utilizzando una colonna capillare MOPH. <ol><li> Lavare la colonna con 100 ml di una miscela 4: 1 di acetonitrile contenente un acido trifluoroacetico 0,1% per 10 minuti a una velocità di flusso di 1 ml / min. Pompa la digestione delle proteine ​​attraverso la colonna, 2 microlitri / min per 30 min. </li><li> Lavare i peptidi non-fosforilati nuovo con una miscela 4: 1 di acetonitrile contenente un acido trifluoroacetico 0,1% per 10 minuti a una velocità di flusso di 1 ml / min. Lavare con acqua per 10 minuti ad una velocità di flusso di 1 ml / min. </li><li> Fosfopeptidi eluire con una soluzione tampone a pH 7 fosfato 250 mM pompato a 1 ml / min per 15 min. Raccogliere il eluente in una fiala e desalt la soluzione con un protocollo standard 19. Preparare un acido / ml 2,5-diidrossibenzoico 2 mg di utilizzarlo come matrice per la spettrometria di matrice laser assistita desorbimento / ionizzazione a tempo di volo di massa (MALDI-TOF-MS). Disegnato 2 ml di acido 2,5-diidrossibenzoico nella punta per eluire il phosphopeptides e individuare direttamente sulla piastra MALDI. </li><li> Analizzare i punti di MALDI-TOF-MS e rigenerare la colonna di lavaggio con acqua e poi il metanolo. </li></ol></li></ol>

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The authors have nothing to disclose.

Il polimero monolite originale contiene gruppi funzionali carbossilici in grado di legarsi ai metalli. Coordinare i siti metallici iniziali sul materiale originale, siamo in grado di crescere un rivestimento PCP (Figura 1A), che incorpora una serie di siti di metallo supplementari plasmare una rete microporosa. Questo rende i materiali MOPH presentati attraenti per procedure di estrazione o di purificazione in cui sono coinvolti specie metalliche, come la tecnica cromatografia di affinità con ioni meta...

Polimeri di coordinazione porosi (PCP) sono composti di coordinazione basato su centri metallici collegati da leganti organici di ripetere le entità di coordinamento che si estendono a 1, 2 o 3 dimensioni che possono essere amorfa o cristallina 1-3. Negli ultimi anni, questa classe di materiali porosi ha attirato l&#39;attenzione diffusa a causa della loro elevata porosità, ampia modulabilità chimica, e la loro stabilità. PCP sono stati esplorati per una vasta gamma di applicazioni, tra cui lo stoccaggio del gas, separazione di gas, e catalisi 3-6, e poco tempo fa, le prime applicazioni analitiche di PCP sono stati descritti 7. A causa delle loro avanzate funzionalità chimica ed alta porosità PCP sono stati presi di mira per il loro enorme potenziale per il miglioramento dei processi di depurazione e separazioni cromatografiche, e un certo numero di segnalazioni relative a questo argomento sono stati pubblicati 7-13. Tuttavia, le prestazioni di PCPs non è attualmente in una equivalelivello nt con materiali cromatografici esistenti probabilmente a causa rapida diffusione attraverso le grandi vuoti interparticellari in letti riempiti di questi solidi a causa della loro morfologia in genere di forma irregolare delle loro particelle o cristalli. Questo imballaggio distribuiti irregolarmente porta ad una minore prestazione del previsto, nonché contropressioni alta colonna e indesiderabili morfologie forma del picco 14,15. Al fine di risolvere il problema della diffusione veloce attraverso i vuoti fra le particelle e contemporaneamente migliorare le prestazioni di PCPs per applicazioni analitiche, lo sviluppo di un materiale ibrida basata su un polimero macroporoso monolite 16 che contiene il PCP sulla superficie dei macropori sarebbe auspicabile. Monoliti di polimeri sono self-contained, materiali pezzo unico in grado di sostenere il flusso convettivo attraverso i pori, che li rende una delle alternative più efficienti da bordare imballaggi e sono stati commercializzati con successo da diversi c<html> ompanies 17,18. Monoliti polimeri porosi sono generalmente basati sulla polimerizzazione di un monomero e un reticolante in presenza di porogens, tipicamente miscele binarie di solventi organici. I materiali monolitici ottenuti hanno una struttura microglobular e un&#39;elevata porosità e permeabilità flusso. Un approccio semplice per unificare questi materiali per preparare un monolito polimero contenente un PCP si basa sulla aggiunta diretta di PCPs as-sintetizzati nella miscela di polimerizzazione del monolito. Questo approccio provocato PCPs principalmente sepolto entro un scaffold polimerico, e non essere attivi per l&#39;ulteriore applicazione del materiale finale 14,15. Un diverso approccio sintetico è chiaramente necessaria per, per esempio, sviluppare film uniformi di PCP, o strutture metallo-organici cristallini (MOF) dove la maggior parte dei pori contenute all&#39;interno del cristallo sono accessibili dal macropori del monolite polimero. t &quot;&gt; Qui riportiamo un semplice protocollo per la preparazione di un materiale polimerico ibrido metallo-organici (MOPH) basato su un supporto polimerico macroporoso con gruppi funzionali adatti per il fissaggio di PCPs, che possono essere facilmente implementati come un self-contained singola -piece monolite polimero in un formato colonna con proprietà ottimali per applicazioni a flusso continuo. La procedura di sintesi del polimero è seguita da una soluzione semplice basata temperatura ambiente &#160; metodo per coltivare un rivestimento PCP sulla superficie interna dei pori del monolite 19-20. Come primo esempio, si descrive la preparazione di un ferro da stiro (III) benzenetricarboxylate (FeBTC) film polimerico coordinamento all&#39;interno di un poli macroporoso (acido stirene-divinilbenzene-metacrilico) monolite. Questo metodo è efficace per la preparazione di polveri all&#39;ingrosso così come colonne capillari e il protocollo descritto è facilmente implementabile ad altri PCP. Come esempio delle potenzialità di MOPHs come materiali funzionali per flow-throuapplicazioni gh, abbiamo applicato il sviluppato FeBTC MOPH che contiene un denso strato di Fe (III) centri per arricchire phosphopeptides da miscele proteiche digeriti sfruttando l&#39;affinità di legame di fosfopeptidi a Fe (III). Il protocollo sviluppato 21 comprende tre parti principali: Preparazione del supporto macroporoso monolite polimero organico; la crescita del rivestimento PCP sulla superficie dei pori del monolite; applicazione per l&#39;arricchimento di fosfopeptidi.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Polyimide-coated capillaries</td>
			<td>Polymicro Technologies</td>
			<td>TSP100375</td>
			<td>100 &#956;m i.d.</td>
		</tr>
		<tr>
			<td>3-(trimethoxysilyl)propyl methacrylate, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>440159</td>
			<td></td>
		</tr>
		<tr>
			<td>Styrene, 99%</td>
			<td>Sigma-Aldrich</td>
			<td>W323306</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>Divinylbenzene, 80%</td>
			<td>Sigma-Aldrich</td>
			<td>414565</td>
			<td></td>
		</tr>
		<tr>
			<td>Methacrylic acid, 98%</td>
			<td>Mallinckrodt</td>
			<td>MK150659</td>
			<td></td>
		</tr>
		<tr>
			<td>Toluene, &#8805;99.5%</td>
			<td>EMD chemicals</td>
			<td>MTX0735-6</td>
			<td></td>
		</tr>
		<tr>
			<td>Isooctane, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>650439</td>
			<td></td>
		</tr>
		<tr>
			<td>2,2&#39;-azobisisobutyronitrile, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>441090</td>
			<td></td>
		</tr>
		<tr>
			<td>Aluminium oxide (basic alumina)</td>
			<td>Sigma-Aldrich</td>
			<td>199443</td>
			<td></td>
		</tr>
		<tr>
			<td>Iron (III) chloride hexahydrate, 97%</td>
			<td>Sigma-Aldrich</td>
			<td>236489</td>
			<td></td>
		</tr>
		<tr>
			<td>1,3,5-benzenetrycarboxylic acid, 95%</td>
			<td>Sigma-Aldrich</td>
			<td>482749</td>
			<td></td>
		</tr>
		<tr>
			<td>Acetonitrile, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>360457</td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium bicarbonate, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>9830</td>
			<td></td>
		</tr>
		<tr>
			<td>Trifluoroacetic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>302031</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol, &#8805;99.8%</td>
			<td>Sigma-Aldrich</td>
			<td>2854</td>
			<td></td>
		</tr>
		<tr>
			<td>Iodoacetamide, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>I1149</td>
			<td></td>
		</tr>
		<tr>
			<td>Dithiothreitol, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>43819</td>
			<td></td>
		</tr>
		<tr>
			<td>Monobasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71505</td>
			<td></td>
		</tr>
		<tr>
			<td>Dibasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71643</td>
			<td></td>
		</tr>
		<tr>
			<td>Phosphoric acid, &#8805;85%</td>
			<td>Sigma-Aldrich</td>
			<td>438081</td>
			<td></td>
		</tr>
		<tr>
			<td>2,5-dihydroxybenzoic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>85707</td>
			<td></td>
		</tr>
		<tr>
			<td>Trypsin</td>
			<td>Sigma-Aldrich</td>
			<td>T8003</td>
			<td>Bovine pancreas</td>
		</tr>
		<tr>
			<td>&#946;-casein</td>
			<td>Sigma-Aldrich</td>
			<td>C6905</td>
			<td>Bovine milk</td>
		</tr>
		<tr>
			<td>ZipTip pipette tips</td>
			<td>Merck Millipore</td>
			<td>ZTC18S096</td>
			<td>C18 resin</td>
		</tr>
	</tbody>
</table>

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.

Una illustrazione schematica della crescita PCP sulla superficie dei pori del monolito polimero organico è mostrato in Figura 1. In questa figura, illustriamo iniziale Fe (III) atomi trattenuti sulla superficie dei pori del polimero monolite originale coordinato ai gruppi funzionali carbossilici . Utilizzando il protocollo qui descritto aggiuntivo legante organico e Fe (III) ioni vengono aggiunti alla superficie, modellare una rete di coordinamento porosa all&#39;interno del monolite polimero. ...

Watch this Scientific Journal Video about Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides at JoVE.com

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

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.

Preparazione di altamente poroso Coordinamento rivestimenti polimerici su macroporosi Polymer Monoliti di avanzata Arricchimento fosfopeptidi

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

preparation-highly-porous-coordination-polymer-coatings-on

Research

JoVE Journal

Chemistry

10.0K Views.  E. O. Lawrence Berkeley National Laboratory. 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.

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

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

Imaging confocale di confinati riposo e fluenti miscele colloidali e polimeri

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

Ricerca

Chimica

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 ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

Terapia fotodinamica con Blended Condurre Polimero / Fullerene nanoparticelle fotosensibilizzanti

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

Preparazione di macroporosi Epitassiali Films quarzo su silicio da Solution Chemical Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

Funzionalizzazione di single-walled nanotubi di carbonio con termo-reversibili Block Copolimeri e caratterizzazione da piccolo angolo Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

La preparazione e la proprietà di Thermo-reversibile reticolato Chimica Gomma Via Diels-Alder

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Monitoring the Effects of Illumination on the Structure of Conjugated Polymer Gels Using Neutron Scattering

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and absence of white light exposure. By instituting a controlled temperature ramp, the gelation of these materials can be precisely monitored as they proceed through this structural evolution, which effectively mirrors the conditions experienced during the solution deposition phase of organic electronic device fabrication. Using small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) along with appropriate fitting protocols we quantify the evolution of select structural parameters throughout this process. Thorough analysis indicates that continued light exposure throughout the gelation process significantly alters the structure of the ultimately formed gel. Specifically, the aggregation process of poly(3-hexylthiophene-2,5-diyl) (P3HT) nano-scale aggregates is negatively affected by the presence of illumination, ultimately resulting in the retardation of growth in conjugated polymer microstructures and the formation of smaller scale macro-aggregate clusters.

A protocol for the analysis of gels formed from the optoelectronic conjugated polymer poly(3-hexylthiophene-2,5-diyl) (P3HT) using small and ultra-small angle neutron scattering in both the presence and absence of illumination is presented.

Monitoraggio degli effetti di illuminazione sulla struttura del gel di polimeri coniugati utilizzando lo Scattering di neutroni

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

A secco microfluidic-spinning e caratterizzazione delle fibre rigenerate seta Fibroin

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

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). ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

Tempo-risolta caratterizzazione fotofisica di tripletto-raccoglitrici composti organici a un utilizzo di ambiente privo di ossigeno un iCCD telecamera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...