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

GMS hazırlanması 1. <ol><li> Alınan Aşağıdaki süreçte tüm kimyasalları kullanın. </li><li> Hidroklorik asit (HCl) çözeltisi 2 M 75 mi hazırlayın. Poli (etilen glikol) 2.0 g tartılır -blok-poli (propilen glikol) -blok-poli (etilen glikol) (P123, molekül ağırlığı = 5,800) ve 2 M HCI çözeltisi hazırlanır, 75 ml içine aktarın. P123 tamamen eriyene kadar oda sıcaklığında, 350 dev / dk bir hızda çözeltiye, manyetik karıştırma uygulanır. Çözelti açık olacaktır. </li><li> Küçük bir şişe ve transfer Bis 180 ul tetraetoksisilan, 4 g (TEOS, MW = 208,33) tartılır [3- (trietoksisilil) propil] -tetrasulfide (TESPTS, MW = 538,94) şişenin içine. Yavaşça şişe iki kimyasal karıştırmak için sallayın. Diğer bir ampul içinde, chloroauric asit 38 mg (HAuCl 4, 99.90%) ağırlığında ve Dİ su, 1 ml içinde çözülür. </li><li> Termokupl tarafından kontrol edilen sıcaklıkta bir yağ banyosunda 35 ° C&#39;ye kadar P123 çözelti sıcaklığının artırılması. </li><li> Ekle TEOS karışımın tümü veTESPTS P123 çözeltisine aşama 1.3 &#39;de hazırlanan ve 700 r / dak kuvvetlice manyetik karıştırma ile çözelti tutun. 2 dakika karıştırıldıktan çözüm tutun, daha sonra 30 saniye içinde adım 1.3 damla damla hazırlanan HAuCl 4 çözeltisi, tüm ekleyin. </li><li> 35 ° C&#39;de 24 saat süre ile 700 devir / dakika ile karıştırılmıştır çözüm tutun. </li><li> 24 saat sonra, 72 saat boyunca 100 ° C&#39;ye ayarlanmış bir fırın içinde kapalı bir şişe deposuna çözeltisi aktarın. Bu hidrotermal işlem denir. </li><li> Hidrotermal işlem sonra HCI kalan çıkarmak için, su ile iki kere ve etanol yıkaması, ardından bir huni altında üç kez 1. filtrasyon kağıt ve negatif basınç çözelti filtre. Her yıkama işlemi sırasında, katı üstünde su veya etanol 1 cm ekleyebilir ve malzeme kurumasını bekleyin. </li><li> 4 saat boyunca 550 ° C &#39;de, bir seramik pota ve kalsine edilmesi için filtreleme ile çökelmesini aktarın. Şöyle rampa programı ayarlayın: 25 ° C 550 ° C arasında, 2 saat için 4, 550 ° C &#39;de devamsaat, daha sonra sıcaklık 40 ° C&#39;nin altına düşene kadar kapı kapalı numune fırın içinde kalmasını sağlar. </li><li> Tavlamadan sonra plastik bir spatula ile, bir cam şişeye aktarın. Sentezlenen malzeme kırmızı renge sahiptir. </li></ol> 2. Katalitik reaksiyon, benzil alkol oksidasyonu <ol><li> Benzil alkol oksidasyonu ayrı çözücü olmaksızın, bir sıvı faz reaksiyonu, ölçü 5 benzil alkol (% 99.8) ile yıkanır ve 25 ml&#39;lik üç boyunlu bir şişeye transfer olduğu için, daha sonra GMS katalizörü 10 mg ağırlığında ve benzil ekle Alkol. </li><li> Reaksiyon sıcaklığının hassas ve düzgün kontrolü sağlamak için manyetik karıştırma ile bir sıcaklık kontrollü yağ banyosu ayarlayın. </li><li> Yağ banyosu içine benzil alkol ve katalizör ile balon koyun, daha sonra 100 ° C&#39;ye kadar sıcaklığa ayarlanmış ve 150 R / dakika karıştırılır. </li><li> Bir kütle akışı kontrolörü ile kontrol 2 ml / dk bir şişeye% 99.9 saflıkta oksijen gaz akışı. </li><li> Ne zamanYağ banyosunun sıcaklığı üç boyunlu bir şişe içine oksijen gazı tanıtmak, 100 ° C&#39;ye ulaşır ve stabilize eder. </li><li> Oksijen akış hızı ve sıcaklığı sabit tutmak, ve reaksiyon, 6 saat devam etmesine izin verir. </li><li> Tepkimeden sonra, bir # 1 filtre kağıdı ile filtre ürünü. Sıvı fazı toplayın ve gaz kromatografisi (GC), bir şişeye bir kısım aktarın. GC şişe içinde (örneğin, 36 ul numune ve 144 ul asetik asit kullanılır.) Her bir kısım örnek için dört parça HPLC dereceli asetik asit karışımı analiz için bir gaz kromatograf otomatik örnekleyici ile şişe yerleştirin. DI su ve etanol ile filtre kağıdı üzerinde, katı bir çözelti yıkayın, sonra hava içinde kurumaya bırakın. Geri dönüştürülmüş katalizör olarak bir spatula ile kurutulmuş katı toplamak. </li><li> Geri dönüşümlü katalizör üç kez 2.7 ile adım 2.3 aynı deney işlemi tekrarlayın. Her bir tekrar olarak, aşama 2.2&#39;de tanımlanan oranı ile eşleşecek şekilde benzil alkol miktarını ayarlar. </li></ol> 3. TherTermal stabilitesi Testi için GMS&#39;nin mal Tedavisi <ol><li> Sentezlenen GMS üç ayrı 300 mg bölümlerini tartılır ve cam şişelerde saklayın. Bunlar toplu 1, kontrol grubu olarak parti 2 ve parti 3. Keep toplu 1 olarak işaretlenmiş ve ısıl işlem için bir fırına toplu 2 ve toplu 3. konur. </li><li> 400 ° C &#39;de işleme aşağıda fırın Programı: 400 ° C, 25 ° C ile rampa 0.5 saat içinde, 4 saat süre ile 400 ° C&#39; de muhafaza Örnek kapı ile fırın içinde kalmasına izin sıcaklık düşme kadar kapalı 40 ° C&#39;nin altında. Bir potada toplu 2 koyun ve programı başlatın. </li><li> 650 ° C&#39;de işleme aşağıda fırın Programı: Kapı kapalı sıcaklığı altına düşene kadar 650 ° C&#39;ye kadar 25 ° C ila rampa 0.75 saat içinde, 4 saat süre ile 650 ° C &#39;de muhafaza, örnek fırın içinde kalmasına izin 40 ° C. Bir potada toplu 3. koyun ve programı başlatın. </li></ol> 4. KarakterizasyonuGMS Malzemelerin 21,22 arasında <ol><li> 60 dakika boyunca 90 ° C ve 480 dakika daha sonra, 350 ° C: fiziksel adsorpsiyon cihazı üzerinde, gazını, aşağıdaki program ile malzeme GMS. Fiziksel adsorpsiyon verileri elde etmek degased malzemeler üzerinde tam izoterm analizi çalıştırın. </li><li> 200 meş holey karbon TEM ızgara üzerinde GMS örnek dağıtın ve bir transmisyon elektron mikroskobu altında örnek görüyoruz. Malzemeyi korumak için 44,000X altında büyütme kısıtlayın. </li><li> Cu Ka radyasyonu (λ = 1,5418 Å) ile çalıştırın XRD. Set 45 kV tüp voltajı ve 40 mA tüp akımı. 0.008 ° &#39;lik bir adım boyutuna ve her adımda 5 saniye kadar bir ölçüm süresine sahip 2θ aralığında ° 10 ° ve 90 yoğunluğunun toplayın. </li></ol>

<ol>
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The authors have nothing to disclose.

Sentez protokolü içinde, yüzey aktif madde konsantrasyonu, çözelti ve reaksiyon sıcaklığı, pH dikkat GMS başarılı bir şekilde oluşması için gereklidir. kritik adımlar 1.2, 1.3, 1.4 ve 1.6 bulunmaktadır. Yukarıda belirtilen parametreler, yüzey aktif oluşan misellerin kritik paketleme parametresi ve faz kontrol eder. misel faz ve morfolojisi GMS için çerçeve olarak hizmet veren silika matris, son durumunu belirler. Ayrıca oluşum sürecinde önemli bir dizisi ve HAuCl çözeltisi ekleme zamanı. T...

Kataliz uygulamaları büyük bir potansiyele sahip gelişmekte olan bir teknoloji olduğu gibi, nano ölçekli malzemeler geçmiş yıllarda yoğun araştırma ilgi aldık. Nano ölçekli katalizörleri rapor arasında, örneğin, Au, Ag, Pd ve Pt gibi soy metal katalizörler, dünya çapında önem 1-3 çekmiştir. Seçin katalitik reaksiyonlar Au ile ilgili Pt, Pd Heck katalizörler üzerinde reaksiyonu ve su bölme karbon monoksit araştırmacıların oksidasyonunu içerir. Gelecek vaat eden bir katalitik potansiyeline rağmen, nano ölçekli altın bağlı zehirlenme, koklaştırma, termal bozulma ve sinterlemeden ve kapatma uygulanabilirliği sınırlıdır. Bu soylu metaller için bir temsilcisi olarak, yüksek seçiciliğe sahiptir ve daha az metal liçi eğilimli, aşırı oksidasyon ve 4. kendini zehirlediğini, yani altın bildirilmiştir. Bununla birlikte, altın katalitik performansı kuvvetli partikül büyüklüğüne bağlıdır. Haruta ve diğ., Katalitik performansı ve gitmek arasındaki ilişkiyi bildirdild kümesi çap, partikül büyüklüğü 2.7 mil 5 ~ altın katalizörlerin en yüksek faaliyeti gösteren. soy metallerin parçacık boyutu hazırlama yöntemi 6-9 ile kontrol edilebilir; Ancak, geniş bir uygulama yolunda önemli engel toplama ve etkinlik kaybı kalır. Sinterleme problemini çözmek için, ortak bir yöntem, bir destek malzemesi üzerinde, nano ölçekli parçacıkların hareketsiz etmektir. Çeşitli destek malzemeleri, gözenekli silis, 10-11, yan iletken metal oksitler, 12-13, polimer 14, grafen 15 ve karbon nanotüplerin 16 de dahil olmak üzere tatbik edilmiştir. Bu termal ve kimyasal olarak kararlı, nispeten atıl, sadece hafif asidiktir ve çok iyi tanımlanmış mezo / mikro-gözenekli hazırlanabilir için kullanılan malzemeler arasında, gözenekli silika destek olarak çekici bir maddedir. gözenekli yapı, metal parçacıklar için iyi destek sağlar, aynı zamanda boyut seçici substrat erişimi verirmetali katalizörleri. Bu seçicilik, çünkü, bu gözenekli malzemeler ile bağlantılı Ayarlanabilirliğin özellikle uygun olduğu görülmüştür. Çoğu zaman, altın partikülleri ve böylece zor silis 19 Altın nano parçacıklar hazırlamak daha silis yüzeyleri 17-18 derece hareketli olması ve hali hazırda yüksek sıcaklıklara maruz bırakıldığında çok büyük (50 + nm) reaktif olmayan partiküller oluşturmak bulunmuştur. Mukherjee vd. 3-aminopropil-trimetoksisilan ve 3-merkaptopropil-trietoksisilan ve desteklenen altın nano partiküller ile gözenekli silis MCM-41 tekil dağılımlı altın nanopartiküllerinin rapor immobilizasyon hidrojenasyon reaksiyonları için son derece etkin olduğu bulunmuştur ve altın bir ayrıştırma bulunmuştur Reaksiyonun 20. Gözenekli silis yüzey modifikasyonu rapor sonra, bir altın hazırlamak için bir yöntem gözenekli silis (GMS) duvarına arakatkılanan bildirilmiştir. Ayrıca, gözenekli silis desteklenen yaklaşım ölçeklenebilir ap sunuyoriçin yaklaşım, potansiyel olarak bağımsız katalizör ve gözenekli bir ortam değiştirmek. Katalitik işlemler hayati ekonomik öneme sahip olduğundan, faydaları çok kapsamlıdır olabilir. geliştirebilme &quot;yeşil&quot; katalizörler çevre üzerinde derin olumlu etkiye sahip ve önemli endüstriyel proseslerin ekonomik fizibilite ve kaynak verimliliğini artıracak.

<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

Umut verici bir katalitik olarak aktif nano reaktör olarak, gözenekli silis (GMS) içinde araya altın nanopartikülleri başarılı bir şekilde sentezlendi ve malzeme özellikleri incelendi. Biz gözenekli silika duvarlarında altın nano parçacıkları birleştirmek için bir pot sol-jel yaklaşımı kullanılır. Sentezi ile başlamak için, P123 miseller oluşturmak için şablon olarak kullanıldı. Daha sonra TESPTS altın nano parçacıkları birleştirmek için bir yüzey modifikasyon maddesi olarak kullanılmıştır. Bu işlemden sonra, TEOS asit ortamında bir polimerizasyon sürecinden bir silis kaynağı olarak ilave edildi. Hidrotermal işleme ve kalsinasyon sonra, nihai ürün satın alındı. Çeşitli teknikler altın interkalasyonlu gözenekli silika gözenekliliği, morfolojisi ve yapısı karakterize etmek yararlanılmıştır. Sonuçlar, altın interkalasyon sonra gözenekli bir silis, kararlı bir yapı göstermiştir. Bir kriter tepki olarak benzil alkolün oksidasyonu sayesinde, GMS malzemeleri yüksek seçimini gösterdibilirlik ve geri dönüşüm.

Bu yöntem, kanser (HCC4017) akciğer hücrelerine karşı normal (HBEC30KT) &#39;de hema sentez seviyesini karşılaştırmak için kullanıldı. 2, normal akciğer hücrelerinin (HBEC30KT) kıyasla kanser hücreleri (HCC4017)&#39; de hema sentez yüksek seviyede göstermektedir. hema sentezi seviyesi, aynı zamanda mitokondriyal uncoupler karbonil siyanit 3-klorofenilhidrazon (CCCP) varlığında, normal ve kanserli hücrelerde ölçülmüştür. Hücreler, heme sentez seviyelerinin ?...

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.

Sentezi ve Mezogözenekli Silika Walls Altın interkalasyonlu Katalitik Performans

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

10.0K Görüntüleme.  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.

Ultra Performanslı Sıvı Kromatografisi ile Bileşimsel Analiz için Bakteriyel Hücre Duvarlarının İzolasyonu ve Hazırlanması

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 ...

Kimya

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).

Enzimatik, kimyasal (Metilasyon) ve Fiziksel (Kütle Spektrometre, Nükleer Manyetik Rezonans) Teknikleri Kullanarak Bitki Duvar heteroksilanlar sıralanması

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.

Protein Bioconjugatlar sentezi<em&gt; yoluyla</em&gt; Sistein-maleimid Kimya

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.

Altın nanorods hidrokinon Esaslı Sentezi

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.

palladyum<em&gt; K</em&gt; -Heterosiklik Karben Kompleksleri: Benzimidazolyum Tuzlarından Sentez ve Karbon-karbon Bağ Oluşturma Reaksiyonlarında Katalitik Aktivite

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.

Platin-nikel Nanowires ve oksijen azaltma performansı için en iyi duruma getirme sentezi

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.

Nb2O5 sentezi için kimyasal yağış yöntemi toplu nikel katalizör yüksek belirli yüzey alanı ile modifiye

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.

Hızlı Nanoprobe sinyal geliştirme içinde in Situ altın nanoparçacık sentezi tarafından

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.

Amphiphilik altın nanopartiküller sentezi ve karakterizasyonu

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.