The authors acknowledge National Science Foundation grant CHE- 1214068 for supporting this research project.

1. Preparazione di GMS <ol><li> Utilizzare tutte le sostanze chimiche nel processo seguente come ricevuto. </li><li> Preparare 75 ml di 2 M di soluzione di acido cloridrico (HCl). Pesare 2,0 g di poli (glicole etilenico) -block-poli (glicole propilenico) -block-poli (glicole etilenico) (P123, MW = 5.800) e trasferire nel preparato 75 ml di soluzione 2 M HCl. A RT, applicare agitazione magnetica alla soluzione ad una velocità di 350 giri / min fino P123 è completamente sciolto. La soluzione sarà limpida. </li><li> Pesare 4 g di tetraetossisilano (TEOS, PM = 208,33) in una piccola fiala e trasferire 180 ml di bis [3- (trietossisilil) propil] -tetrasulfide (TESPTS, PM = 538,94) nel flaconcino. Agitare lentamente il flacone per miscelare le due sostanze chimiche. In un altro flacone, pesare 38 mg di acido cloroaurico (HAuCl4, 99,90%) e si dissolvono in 1 ml di acqua deionizzata. </li><li> Aumentare la temperatura della soluzione P123 a 35 ° C in un bagno d&#39;olio con temperatura controllata da termocoppia. </li><li> Aggiungere tutta la miscela di TEOS eTESPTS preparata al punto 1.3 alla soluzione P123, e mantenere la soluzione a vigorosa agitazione magnetica di 700 giri / min. Mantenere la soluzione mescolando per 2 minuti, quindi aggiungere tutti HAuCl4 soluzione preparata al punto 1.3, goccia a goccia in 30 secondi. </li><li> Mantenere la soluzione sotto agitazione a 700 giri / min per 24 ore a 35 ° C. </li><li> Dopo 24 ore, trasferire la soluzione in una bottiglia sigillata e conservare in forno a 100 ° C per 72 ore. Questo è chiamato trattamento idrotermale. </li><li> Dopo il trattamento idrotermico, filtrare la soluzione con una carta # 1 filtrazione e pressione negativa in un imbuto, poi lavare con acqua due volte e etanolo tre volte per rimuovere residuo HCl. Nel corso di ogni processo di lavaggio, aggiungere acqua o etanolo 1 cm sopra solida e attendere che il materiale si asciughi. </li><li> Trasferire precipitazione da filtrazione crogiolo ceramico e calcinato a 550 ° C per 4 ore. Impostare il programma rampa come segue: 25 ° C a 550 ° C per 2 ore, mantenere a 550 ° C per 4hr, quindi permettere al campione di rimanere nel forno con la porta chiusa fino a quando la temperatura scende al di sotto di 40 ° C. </li><li> Dopo calcinazione, trasferire il prodotto ad una fiala di vetro con una spatola di plastica. Il materiale sintetizzato ha un colore rosso. </li></ol> 2. Reazione catalitica, ossidazione di alcool benzilico <ol><li> Poiché l&#39;ossidazione di alcool benzilico è una reazione in fase liquida senza solventi separata, misura 5 ml di alcool benzilico (99,8%) e trasferirlo in un pallone da 25 ml a tre colli, si pesa 10 mg di GMS catalizzatore e aggiungere al benzile alcol. </li><li> Impostare un bagno d&#39;olio a temperatura controllata con agitazione magnetica per assicurare il controllo preciso e uniforme della temperatura di reazione. </li><li> Mettere il pallone con alcool benzilico e il catalizzatore nel bagno d&#39;olio, quindi impostare la temperatura a 100 ° C e agitare a 150 giri / min. </li><li> Flusso di gas di ossigeno con il 99,9% di purezza nel pallone a 2 ml / min controllati da un controllore di flusso di massa. </li><li> Quando iltemperatura del bagno ad olio raggiunge 100 ° C e si stabilizza, introdurre gas ossigeno nel pallone a tre colli. </li><li> Mantenere costante la portata di ossigeno e la temperatura, e lasciare che la reazione proceda per 6 ore. </li><li> Dopo la reazione, filtrata del prodotto con una carta # 1 filtrazione. Raccogliere la fase liquida e trasferire una parte in una gascromatografia (GC) flaconcino. Nella fiala GC, mescolare acido acetico quattro parti HPLC grado per ogni campione da una parte (ad esempio, utilizzare 36 ml del campione e 144 ml di acido acetico.) Posizionare il flaconcino su una auto campionatore gascromatografo per l&#39;analisi. Lavare il precipitato solido sulla carta da filtro con acqua deionizzata ed etanolo poi lasciare asciugare all&#39;aria. Raccogliere il solido essiccato con una spatola come catalizzatore riciclato. </li><li> Ripetere la stessa procedura esperimento dal punto 2.3 a 2.7 con catalizzatore riciclato tre volte. In ogni ripetizione, regolare la quantità di alcool benzilico per abbinare il rapporto descritto al punto 2.2. </li></ol> 3. Thermal Trattamento di GMS per il test di stabilità termica <ol><li> Pesare tre distinte porzioni 300 mg di GMS sintetizzati, e conservarli in fiale di vetro. Questi sono contrassegnati come lotto 1, lotto 2 e lotto 3. Tenere lotto 1 come gruppo di controllo, e mettere dei lotti 2 e lotto 3 in una fornace per trattamento termico. </li><li> Programma del forno come segue per la lavorazione a 400 ° C: rampa da 25 ° C a 400 ° C in 0,5 ore, mantenere a 400 ° C per 4 ore, consentire il campione di rimanere nel forno con la porta chiusa fino cascate temperatura sotto i 40 ° C. Mettere lotto 2 in un crogiolo e avviare il programma. </li><li> Programma del forno come segue per la lavorazione a 650 ° C: rampa da 25 ° C a 650 ° C in 0,75 ore, mantenere a 650 ° C per 4 ore, consentire il campione di rimanere in forno con la porta chiusa fino a quando la temperatura scende sotto 40 ° C. Mettere lotto 3 in un crogiolo e avviare il programma. </li></ol> 4. Caratterizzazionedei materiali GMS 21,22 <ol><li> Sullo strumento fisisorbimento, degassare GMS materiali con il seguente programma: 90 ° C per 60 minuti e poi a 350 ° C per 480 min. Eseguire un&#39;analisi completa-isoterma sui materiali degassificata per ottenere i dati fisisorbimento. </li><li> Disperse campione GMS su una griglia TEM carbonio 200 mesh holey e osservare il campione al microscopio elettronico a trasmissione. Limitare ingrandimenti in 44,000X per proteggere il materiale. </li><li> XRD Corri con radiazione Cu Kα (λ = 1,5418 Å). Set tensione del tubo di 45 kV, e la corrente del tubo di 40 mA. Raccogliere intensità nell&#39;intervallo 2θ tra 10 ° e 90 ° con un passo di 0,008 ° e un tempo di misura di 5 sec ad ogni passo. </li></ol>

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The authors have nothing to disclose.

Nel protocollo di sintesi, l&#39;attenzione alla concentrazione di tensioattivo, pH della soluzione di reazione e la temperatura è fondamentale per la formazione di successo di GMS. I passaggi critici sono 1.2, 1.3, 1.4 e 1.6. I suddetti parametri controllano il parametro imballaggio critica e la fase di micelle formate da tensioattivo. La fase e la morfologia del micelle determina lo stato finale della matrice di silice, che funge da quadro per GMS. Altrettanto importante nel processo di formazione è la sequenza e il...

Come una tecnologia emergente che ha un grande potenziale nelle applicazioni di catalisi, materiali su scala nanometrica hanno ricevuto l&#39;interesse intensa attività di ricerca negli ultimi decenni. Tra i catalizzatori nanoscala segnalati, catalizzatori di metalli nobili, come Au, Ag, Pd e Pt hanno attirato l&#39;attenzione in tutto il mondo 1-3. Seleziona reazioni catalitiche includono l&#39;ossidazione dei ricercatori di monossido di carbonio su Au, Heck reazione catalizzatori Pd, e la scissione dell&#39;acqua con Pt. Nonostante il potenziale catalitico promettente, oro nanoscala è limitata nella sua applicazione a causa della disattivazione di avvelenamento, coking, degradazione termica, e sinterizzazione. E &#39;stato riportato che l&#39;oro, come rappresentante per metalli nobili, ha l&#39;alta selettività ed è meno soggetto a lisciviazione metallo, over-ossidazione, e di auto-avvelenamento 4. Tuttavia, la prestazione catalitica di oro dipende fortemente dalla granulometria. Haruta et al. Ha riportato il rapporto tra prestazioni catalitiche e andarediametro grappolo ld, dimostrando la più alta attività di catalizzatori oro con granulometria ~ 2.7 nm 5. La dimensione delle particelle di metalli nobili può essere controllato dal metodo di preparazione 6-9; Tuttavia, il principale ostacolo verso un&#39;ampia applicazione rimane aggregazione e perdita di attività. Per risolvere il problema di sinterizzazione, un metodo comune è quella di immobilizzare nanoparticelle su un materiale di supporto. Vari materiali di supporto sono state applicate compresa la silice porosa 10-11, ossidi metallici semiconduttori 12-13, polimeri 14, grafene 15 e nanotubi di carbonio 16. Tra i materiali impiegati, silice porosa è un materiale attraente come un supporto perché è solo leggermente acido, relativamente inerte, termicamente e chimicamente stabile, e può essere preparata con molto ben definito meso / microporosità. La struttura porosa fornisce un buon supporto per particelle di metallo, ma conferisce anche accesso dimensione substrato selettivoi catalizzatori metallici. Questa selettività è particolarmente promettente per la tunability associato con questi materiali porosi. Spesso, particelle d&#39;oro si trovano ad essere estremamente mobile su superfici silice 17-18 e facilmente formare molto grandi (50+ nm) particelle reattivi quando esposto a temperature elevate, rendendo così difficile preparare nanoparticelle di oro su silice 19. Mukherjee et al. Segnalato l&#39;immobilizzazione di nanoparticelle d&#39;oro monodisperse su mesoporosi silice MCM-41 da 3 amminopropil-trimetossisilano e 3-mercaptopropil-trietossisilano, e le nanoparticelle d&#39;oro supportati sono risultati essere molto attivo per reazioni di idrogenazione e stata trovata nessuna lisciviazione dell&#39;oro nella reazione 20. A seguito della relazione di modifica della superficie della silice mesoporosa, abbiamo riportato un metodo per preparare oro intercalati nella parete della silice mesoporosa (GMS). Inoltre, l&#39;approccio di silice mesoporosa supportato offre un ap scalabileproccio potenzialmente modificare autonomamente il catalizzatore e l&#39;ambiente poroso. Dal momento che i processi catalitici sono di vitale importanza economica, i benefici potrebbero essere di vasta portata. La capacità di sviluppare catalizzatori &quot;verdi&quot; avrebbe un profondo impatto positivo sull&#39;ambiente e migliorare la fattibilità e l&#39;efficienza delle risorse economiche di importanti processi industriali.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol)</td>
			<td>Aldrich</td>
			<td>435465-250ML</td>
			<td></td>
		</tr>
		<tr>
			<td>tetraethoxysilane</td>
			<td>TCI</td>
			<td>201-083-8</td>
			<td></td>
		</tr>
		<tr>
			<td>bis[3-(triethoxysilyl)propyl]-tetrasulfide</td>
			<td>GELEST</td>
			<td>SIB1825.0-100GM</td>
			<td></td>
		</tr>
		<tr>
			<td>chloroauric acid</td>
			<td>Aldrich</td>
			<td>520918-1G</td>
			<td></td>
		</tr>
		<tr>
			<td>benzyl alcohol</td>
			<td>Sigma-Aldrich</td>
			<td>305197-1L</td>
			<td></td>
		</tr>
		<tr>
			<td>nitrogen physisorption</td>
			<td>Micromeritics</td>
			<td>Tristar II</td>
			<td></td>
		</tr>
		<tr>
			<td>X-ray diffraction</td>
			<td>Philips</td>
			<td>X&#39;Pert Pro</td>
			<td></td>
		</tr>
		<tr>
			<td>transmission electron microscopy</td>
			<td>Philips</td>
			<td>CM200</td>
			<td></td>
		</tr>
		<tr>
			<td>gas chromatography</td>
			<td>Shimadzu</td>
			<td>GC-2010</td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis and catalytic performance of gold intercalated in the walls of mesoporous silica

Come promettendo reattore nano cataliticamente attivo, nanoparticelle d&#39;oro intercalate in silice mesoporosa (GMS) sono stati sintetizzati con successo e le proprietà dei materiali sono stati studiati. Abbiamo utilizzato un approccio sol-gel una pentola a intercalare nano particelle d&#39;oro nelle pareti di silice mesoporosa. Per iniziare con la sintesi, P123 è stato utilizzato come modello per formare micelle. Poi TESPTS è stato usato come agente modifica superficiale intercalare nano particelle d&#39;oro. A seguito di questo processo, TEOS stato aggiunto come una fonte di silice che ha subito un processo di polimerizzazione in ambiente acido. Dopo trattamento idrotermale e calcinazione, il prodotto finale è stato acquisito. Diverse tecniche sono stati utilizzati per caratterizzare la porosità, la morfologia e la struttura del oro intercalato silice mesoporosa. I risultati hanno mostrato una struttura stabile della silice mesoporosa dopo l&#39;oro intercalazione. Attraverso l&#39;ossidazione di alcool benzilico come reazione di riferimento, i materiali GMS mostrato alta Selectività e la riciclabilità.

Questo metodo è stato utilizzato per confrontare i livelli di sintesi dell&#39;eme nel normale (HBEC30KT) vs. cancro (HCC4017) cellule polmonari. La Figura 2 mostra un più alto livello di sintesi dell&#39;eme nelle cellule tumorali (HCC4017) rispetto alle cellule polmonari normali (HBEC30KT). Il livello di sintesi dell&#39;eme stata anche misurata in cellule normali e tumorali in presenza di cianuro di carbonile mitocondriale disaccoppiatore 3-chlorophenylhydrazone (CCCP). Le cellule sono state tratta...

Watch this Scientific Journal Video about Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica at JoVE.com

Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

Sintesi e prestazioni catalitica dell&#39;oro intercalata nelle Mura di mesoporosi silice

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties ...

synthesis-catalytic-performance-gold-intercalated-walls-mesoporous

Research

JoVE Journal

Chemistry

9.9K Views.  Colorado School of Mines. Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

Video: Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

Isolation and Preparation of Bacterial Cell Walls for Compositional Analysis by Ultra Performance Liquid Chromatography

The bacterial cell wall is critical for the determination of cell shape during growth and division, and maintains the mechanical integrity of cells in the face of turgor pressures several atmospheres in magnitude. Across the diverse shapes and sizes of the bacterial kingdom, the cell wall is composed of peptidoglycan, a macromolecular network of sugar strands crosslinked by short peptides. Peptidoglycan&#8217;s central importance to bacterial physiology underlies its use as an antibiotic target and has motivated genetic, structural, and cell biological studies of how it is robustly assembled during growth and division. Nonetheless, extensive investigations are still required to fully characterize the key enzymatic activities in peptidoglycan synthesis and the chemical composition of bacterial cell walls. High Performance Liquid Chromatography (HPLC) is a powerful analytical method for quantifying differences in the chemical composition of the walls of bacteria grown under a variety of environmental and genetic conditions, but its throughput is often limited. Here, we present a straightforward procedure for the isolation and preparation of bacterial cell walls for biological analyses of peptidoglycan via HPLC and Ultra Performance Liquid Chromatography (UPLC), an extension of HPLC that utilizes pumps to deliver ultra-high pressures of up to 15,000 psi, compared with 6,000 psi for HPLC. In combination with the preparation of bacterial cell walls presented here, the low-volume sample injectors, detectors with high sampling rates, smaller sample volumes, and shorter run times of UPLC will enable high resolution and throughput for novel discoveries of peptidoglycan composition and fundamental bacterial cell biology in most biological laboratories with access to an ultracentrifuge and UPLC.

The bacterial cell wall is composed of peptidoglycan, a macromolecular network of sugar strands crosslinked by peptides. Ultra Performance Liquid Chromatography provides high resolution and throughput for novel discoveries of peptidoglycan composition. We present a procedure for the isolation of cell walls (sacculi) and their subsequent preparation for analysis via UPLC.

Isolamento e preparazione delle pareti cellulari batteriche per l'analisi compositia mediante cromatografia liquida ad alte prestazioni

The bacterial cell wall is critical for the determination of cell shape during growth and division, and maintains the mechanical integrity of cells in the ...

Ricerca

Chimica

Sequencing of Plant Wall Heteroxylans Using Enzymic, Chemical (Methylation) and Physical (Mass Spectrometry, Nuclear Magnetic Resonance) Techniques

This protocol describes the specific techniques used for the characterization of reducing end (RE) and internal region glycosyl sequence(s) of heteroxylans. De-starched wheat endosperm cell walls were isolated as an alcohol-insoluble residue (AIR)1 and sequentially extracted with water (W-sol Fr) and 1 M KOH containing 1% NaBH4 (KOH-sol Fr) as described by Ratnayake et al. (2014)2. Two different approaches (see summary in Figure 1) are adopted. In the first, intact W-sol AXs are treated with 2AB to tag the original RE backbone chain sugar residue and then treated with an endoxylanase to generate a mixture of 2AB-labelled RE and internal region reducing oligosaccharides, respectively. In a second approach, the KOH-sol Fr is hydrolyzed with endoxylanase to first generate a mixture of oligosaccharides which are subsequently labelled with 2AB. The enzymically released ((un)tagged) oligosaccharides from both W- and KOH-sol Frs are then methylated and the detailed structural analysis of both the native and methylated oligosaccharides is performed using a combination of MALDI-TOF-MS, RP-HPLC-ESI-QTOF-MS and ESI-MSn. Endoxylanase digested KOH-sol AXs are also characterized by nuclear magnetic resonance (NMR) that also provides information on the anomeric configuration. These techniques can be applied to other classes of polysaccharides using the appropriate endo-hydrolases.

Sequencing of Plant Wall Heteroxylans Using Enzymic, Chemical Methylation and Physical Mass Spectrometry, Nuclear Magnetic Resonance Techniques

This protocol describes the specific techniques used for the structural characterization of reducing end (RE) and internal region glycosyl sequence(s) of heteroxylans by tagging the RE with 2 aminobenzamide prior to enzymatic (endoxylanase) hydrolysis and then analysis of the resultant oligosaccharides using mass spectrometry (MS) and nuclear magnetic resonance (NMR).

Il sequenziamento di Plant parete Heteroxylans Utilizzando enzimatica, chimica (metilazione) e (Spettrometria di Massa, Risonanza Magnetica Nucleare) tecniche fisiche

This protocol describes the specific techniques used for the characterization of reducing end (RE) and internal region glycosyl sequence(s) of ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the development of antibody drug conjugates (ADCs) and nanomedicine, fluorescent microscopy and systems chemistry. For many of these applications, specificity of the bioconjugation method used is of prime concern. The Michael addition of maleimides with cysteine(s) on the target proteins is highly selective and proceeds rapidly under mild conditions, making it one of the most popular methods for protein bioconjugation.
We demonstrate here the modification of the only surface-accessible cysteine residue on yeast cytochrome c with a ruthenium(II) bisterpyridine maleimide. The protein bioconjugation is verified by gel electrophoresis and purified by aqueous-based fast protein liquid chromatography in 27% yield of isolated protein material. Structural characterization with MALDI-TOF MS and UV-Vis is then used to verify that the bioconjugation is successful. The protocol shown here is easily applicable to other cysteine - maleimide coupling of proteins to other proteins, dyes, drugs or polymers.

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

This protocol details the important steps required for the bioconjugation of a cysteine containing protein to a maleimide, including reagent purification, reaction conditions, bioconjugate purification and bioconjugate characterization.

Sintesi di proteine ​​bioconiugati<em&gt; via</em&gt; Chimica cisteina-maleimmide

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Hydroquinone Based Synthesis of Gold Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the synthetic methods for the preparation of gold nanorods are still not fully optimized. In this paper we describe a new, highly efficient, two-step protocol based on the use of hydroquinone as a mild reducing agent. Our approach allows the preparation of nanorods with a good control of size and aspect ratio (AR) simply by varying the amount of hexadecyl trimethylammonium bromide (CTAB) and silver ions (Ag+) present in the "growth solution". By using this method, it is possible to markedly reduce the amount of CTAB, an expensive and cytotoxic reagent, necessary to obtain the elongated shape. Gold nanorods with an aspect ratio of about 3 can be obtained in the presence of just 50 mM of CTAB (versus 100 mM used in the standard protocol based on the use of ascorbic acid), while shorter gold nanorods are obtained using a concentration as low as 10 mM.

This paper describes a protocol for the synthesis of gold nanorods, based on the use of hydroquinone as reducing agent, plus the different mechanisms for controlling their size and aspect ratio.

Idrochinone Based Sintesi di oro Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. Detailed and generalized protocols are also presented for testing the catalytic activity of such complexes in arylation and Suzuki-Miyaura cross-coupling reactions. Representative results are shown for the catalytic activity of the four complexes in arylation and Suzuki-Miyaura type reactions. For each of the reactions investigated, at least one of the four complexes successfully catalyzed the reaction, qualifying them as promising candidates for catalysis of many carbon-carbon bond-forming reactions. The protocols presented are general enough to be adapted for the synthesis, purification and catalytic activity testing of new palladium N-heterocyclic carbene complexes.

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. The complexes were tested for catalytic activity in arylation and Suzuki-Miyaura reactions. For each reaction investigated, at least one of the four complexes successfully catalyzed the reaction.

Palladio<em&gt; N</em&gt; Complessi di Carbene eterocicliche: Sintesi dei sali di benzimidazolium e attività catalitica in reazioni di formazione di legame di carbonio-carbonio

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

Sintesi di nanofili di platino-nichel e ottimizzazione per le prestazioni di riduzione di ossigeno

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Modificare il metodo di precipitazione chimica per la sintesi di Nb2O5 catalizzatori di nichel Bulk con elevata superficie specifica

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au3+ to Au0. There are several chemical reactions that enable the reduction of Au3+ to Au0. In the protocol, Good&#39;s buffers and H2O2 are used and it is possible to favor the deposition of Au0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

In this work, a protocol for signal enhancement of nanoprobe-based biosensing is presented. The protocol is based on the reduction of chloroauric acid onto the surface of existing nanoprobes that consist of gold, silver, silica or iron-oxide nanoparticles.

Segnale Nanosonda rapido aumento di sintesi di nanoparticelle di oro In Situ

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

Sintesi e caratterizzazione delle nanoparticelle d'oro dell'anfifile

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

Gold Nanoparticle Synthesis

Gold nanoparticles (Au nanoparticles) that are ~12 nm in diameter were synthesized by rapidly injecting a solution of 150 mg (0.15 mmol) of tetrachloroauric acid in 3.0 g (3.7 mmol, 3.6 mL) of oleylamine (technical grade) and 3.0 mL of toluene into a boiling solution of 5.1 g (6.4 mmol, 8.7 mL) of oleylamine in 147 mL of toluene. While boiling and mixing the reaction solution for 2 hours, the color of the reaction mixture changed from clear, to light yellow, to light pink, and then slowly to dark red. The heat was then turned off, and the solution was allowed to gradually cool down to room temperature for 1 hour. The gold nanoparticles were then collected and separated from the solution using a centrifuge and washed three times; by vortexing and dispersing the gold nanoparticles in 10 mL portions of toluene, and then precipitating the gold nanoparticles by adding 40 mL portions of methanol and spinning them in a centrifuge. The solution was then decanted to remove any remaining byproducts and unreacted starting materials. Drying the gold nanoparticles in a vacuum environment produced a solid black pellet; which could be stored for long periods of time (up to one year) for later use, and then redissolved in organic solvents such as toluene.

A protocol for synthesizing ~12 nm diameter gold nanoparticles (Au nanoparticles) in an organic solvent is presented. The gold nanoparticles are capped with oleylamine ligands to prevent agglomeration. The gold nanoparticles are soluble in organic solvents such as toluene.