Yazarlar bu proje için Eğitim Tier 2 Araştırma Fonu Singapur Bakanlığı (proje MOE2013-T2-2-002) fon kabul.

1,3,5-Triphenylbenzene 1. Hazırlama İşlemi (1) <ol><li> Manyetik karıştırıcı, geri akış kondansatörü, nitrojen girişi, kabarcık, damlatma hunisi ve bir termometre ile donatılmış yuvarlak dipli bir üç boyunlu 250 ml&#39;lik bir şişe içine asetofenon karışımı (4.0 g, 33.3 mmol) ve mutlak etanol 100 ml yerleştirin. damlatma hunisi kullanılarak azot altında 0 ° C&#39;de bir kısım halinde karışıma silikon tetraklorür (11.9 g, 8.0 mi, 70.2 mmol, 2.1 eşd.) eklenir. </li><li> 10 dakika süre ile gaz halinde hidrojen klorür evrimi dikkate alınmalıdır. Daha sonra 20 saat boyunca 40 ° C&#39;de, reaksiyon karışımı karıştırılmıştır. </li><li> 23 ° C&#39;ye kadar, reaksiyon karışımı, soğumaya ve buz ile karıştırılmış su 200 g dökün (1: 1 kütle oranı). </li><li> Bir ekstraksiyon hunisi kullanılarak diklorometan (2 x 100 mi) ile elde edilen karışımın ekstrakte edin. </li><li> Doymuş NaCI çözeltisi (100 mi) ve susuz MgSO 4 kuru 15 gr ile bir kez bir araya suyla yıkayın. kapalı sıvı kısmını filtrelemek ve daha sonra bize konsantreBir dönen buharlaştıncı ing. </li><li> 2.2 g (% 63 verim) 1,3,5-triphenylbenzene elde etmek üzere etanolden tekrar kristalleştirme yoluyla ürünün arıtılması (gece boyunca 6 ° C &#39;de tutarak Çözücünün kısmen buharlaştırılmasından ardından etanol az miktarda çözünmesi, ve hızlı filtrasyon) (1), açık sarı kristaller halinde. Not: 1 &#39;H-NMR (400 MHz, CDCI3). Δ = 7.41 (m, 3H), 7.50 (m, 6H), 7.72 (d, 6H, J = 7.33Hz), 7.80 (s, 3H) 13 Cı-NMR (400 MHz, CDCI3): = 125,21, 127,39, 127.57, 128.88, 141.18, 142,38 δ. </li></ol> 2. LiSES 1,3,5-Triphenylbenzene ile hazırlanmıştır <ol><li> 1,3,5-triphenylbenzene tabanlı LiSES hazırlanması NOT: Bu yazıda kullanılan 1,3,5-triphenylbenzene yukarıda açıklanan prosedüre uygun olarak sentezlendi. Li ile ifade edilir 1,3,5-triphenylbenzene merkezli LiSES X LI gösterir TPB (THF) 24.7 x: PAH mol oranı ve TPB 1,3,5-triphenylbenzene gösterir. Li hazırlayınX TPB (THF), aşağıdaki adımları ile, oda sıcaklığında, argon doldurulmuş eldiven kutusu içinde 24.7: <ol><li> Li hedef molar bileşimi TPB (THF), x = 1, 2, 3 ve 4. 41.6 mg, 83.3 mg, 24.7, 124.9 x elde etmek için ayrı ayrı eldiven kutusu içinde, metalik Li, THF ve TPB iyi tanımlanmış miktarlarının ölçümü mg, X = 1, 2, 3 ve 4 için Li 166.6 mg. </li><li> Dört LiSES numunelerin her hazırlanabilir için, her şişe için TPB (THF) 24.7 renksiz çözeltiler 12 ml oluşturacak şekilde dört ayrı cam şişe içinde, THF 12 ml TPB 1.84 g çözülür. Tüm Çözeltilerin 0.5 M 1,3,5-triphenylbenzene kullanın. </li><li> Dört şişe Li folyolar tartılmış metalik ekleyin ve Parafilm ile şişeleri mühür. </li><li> Metalik Li tam olarak çözünmesini sağlamak için, bir cam kaplı manyetik karıştırıcı kullanılarak, her bir şişe gece boyunca karıştırın. </li></ol></li><li> iletkenlik Ölçümleri <ol><li> taşımakDört elektrot tekniğine dayalı standart iletkenlik hücresi sonda kullanılarak bütün iletkenlik ölçümleri. Bir metre hücre probu takın. prob aynı anda çözeltinin sıcaklığını ölçmek ve hem iletkenlik ve sıcaklık ölçümlerini görüntülemek için ikincil bir işlevi vardır. </li><li> Önceki ölçümlere, torpido gözü dışarıda iletkenlik sondanın üreticisi tarafından sağlanan standart 0.01 M sulu KCl çözeltisi 50 ml kullanılarak kalibre. </li><li> 1,3,5-triphenylbenzene tabanlı LiSES için tüm iletkenlik ölçümleri yürütmek, Li TPB (THF) torpido gözünün içine x = 1, 2, 3, 4 için 24.7 x. </li><li> Bu LiSES her biri için, kısa bir cam silindir içine örneği dökmek ve çözüm içine probu batırmayın. ortam sıcaklığında, her örnek döner kadar bir ila iki saat arasında bir süre boyunca iletkenlik ölçümü kaydedin. oda sıcaklığına gelmesi için her bir örnek için geçen süre ~ 1-2 saattir. sonda wHasta iletkenlik ölçüm süresi boyunca numune içine batırılmış durumda tutulabilir. </li></ol></li></ol> 3. Corannulene <ol><li> corannulene bazlı LiSES hazırlanması NOT:. PAH molar: Bu çalışmada kullanılan corannulene çok aşamalı literatür prosedürü kullanılarak fiziksel Okulu ve Matematik Bilimleri, NTU sentezlenmiştir 9 corannulene tabanlı LiSES Li ile gösterilir x Li gösterir Kor (THF) 247 x oranı ve Kor corannulene gösterir. Hazırlama Li, aşağıdaki adımları ile, oda sıcaklığında, argon doldurulmuş eldiven kutusu içinde 247 Kor (THF) x: <ol><li> Li Cor X&#39;in kullanımı 4.2 mg, 8.3 mg, x = 1, 2, 3, 4 ve 5 için 247 (THF), hedef molar bileşimi elde etmek için ayrı ayrı eldiven kutusu içinde, metalik Li, THF ve Kor iyi tanımlanmış miktarlarının ölçümü, 12.5 mg, 16.6 mg ve X = 1, 2, 3, 4 ve 5 için Li 20.8 mg. </li><li> Next, beş LiSES örnekleri de (x = 1, 2, 3, 4 ve 5), beş farklı cam şişe içinde, THF, 12 ml kor 0.15 g çözülür hazırlanacak her biri için Kor renksiz bir çözelti 12 ml oluşturacak şekilde her şişe (THF) 247. ), 0.05 M bir corannulene konsantrasyonu kullanın. </li><li> Sonraki Li Kor (THF) 247 beş şişe folyolar tartılmış metalik ekleyebilir ve Parafilm ile şişeleri mühür. </li><li> metalik lityum tamamen çözülmesini sağlamak için bir cam kaplı manyetik karıştırıcı kullanılarak, her bir şişe gece boyunca karıştırın. </li></ol></li><li> iletkenlik Ölçümleri <ol><li> Sıcaklık ölçümleri karşı iletkenlik sağlamak için, Li Cor (THF), x = 1, 2, 3, 4 ve tek tek eldiven kutusundan 5 için 247 X içeren beş şişe her kaldırma, para-film ile ikinci kat sarın ve batırmak kuru buz dolu yalıtılmış bir Strafor konteyner içinde. NOT: LiSES örnekleri cont gelmedişişeler mühürlü çünkü torpido gözü dışarıda iken nem veya oksijen ya hareket. </li><li> iletkenlik ölçümleri için izolasyon kutusu içine geri aktarılır önce yaklaşık 30 dakika boyunca kuru buz batırılır, her şişe tutarak, yaklaşık 10 ° C&#39;ye kadar, her şişe soğutun. </li><li> Her biri için en az 5 kez yoğunlaşma suyunun hiçbir iz geri torpido gözünün içine şişe eşlik sağlamak için örnek soğutmalı torpido gözünün ön-odasına temizleyin. </li><li> Sıcaklık ölçümleri karşı iletkenliği naftalen tabanlı LiSES örnek 1 için toplanan edildiği şekilde, Li iletkenliğini ölçmek için benzer 247 (x = 1, 2, 3, 4, 5) birinin bir süre boyunca kor (THF) x her numune kadar iki saat çevre sıcaklığında geri döndü. prob iletkenlik ölçüm süresi boyunca numune dalmış kalacaktır. </li></ol></li></ol>

<ol>
	<li>Tan, K. S., Yazami, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physical-Chemical+and+Electrochemical+Studies+of+the+Lithium+Naphthalenide+Anolyte.">Physical-Chemical and Electrochemical Studies of the Lithium Naphthalenide Anolyte.</a> Electrochim Acta. 180, 629-635 (2015).</li><li>Tan, K. S., Grimsdale, A. C., Yazami, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+Characterisation+of+Biphenyl-Based+Lithium+Solvated+Electrons+Solutions.">Synthesis and Characterisation of Biphenyl-Based Lithium Solvated Electrons Solutions.</a> J Phys Chem B. 116, 9056-9060 (2012).</li><li>Rinaldi, A., Tan, K. S., Wijaya, O., Wang, Y., Yazami, R., Menictas, C., Skyllas-Kazacos, M., Lim, T. M., Hughes, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ch.+11.">Ch. 11.</a> Advances in batteries for large- and medium-scale energy storage applications in power systems and electric vehicles. , (2014).</li><li>Wang, Y., Tan, K. S., Yazami, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Materials Challenges In Alternative &amp; Renewable Energy (MCARE 2014). , (2014).</li><li>Yazami, R., Tan, K. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> in 8th annual Li Battery Power. , (2012).</li><li>Yazami, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hybrid+Electrochemical+Generator+With+A+Soluble+Anode.">Hybrid Electrochemical Generator With A Soluble Anode.</a> US patent. , (2010).</li><li>Yazami, R., Tan, K. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Liquid+Metal+Battery.">Liquid Metal Battery.</a> US patent. , (2015).</li><li>Lim, Z. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+assessment+of+new+cyclopenta-2,4-dienone+derivatives+for+energy+storage+applications.">Synthesis and assessment of new cyclopenta-2,4-dienone derivatives for energy storage applications.</a> Synthetic Met. 200, 85-90 (2015).</li><li>Butterfield, A. M., Gilomen, B., Siegel, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kilogram-Scale+Production+of+Corannulene.">Kilogram-Scale Production of Corannulene.</a> Org. Process Res. Dev. 16, 664-676 (2012).</li><li>Elmorsy, S. S., Pelter, A., Smith, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+direct+production+of+tri-+and+hexa-substituted+benzenes+from+ketones+under+mild+conditions.">The direct production of tri- and hexa-substituted benzenes from ketones under mild conditions.</a> Tetrahedron Lett. 32, 4175-4176 (1991).</li><li>Zabula, A. V., Filatov, A. S., Spisak, S. N., Rogachev, A. Y., Petrukhina, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Main+Group+Metal+Sandwich:+Five+Lithium+Cations+Jammed+Between+Two+Corannulene+Tetraanion+Decks.">A Main Group Metal Sandwich: Five Lithium Cations Jammed Between Two Corannulene Tetraanion Decks.</a> Science. 333, 1008-1011 (2011).</li></ol>

Yazarlar ifşa hiçbir şey yok.

1,3,5-triphenylbenzene tabanlı LiSES için, hafif bir rengi olan bir örnek, solvatlanmış elektronlar düşük bir konsantrasyonuna sahip olduğu görülmektedir. Li TPB (THF) 24.7 (x = 1, 2, 3, 4) bifenil ve naftalen 1 yapılan LiSES için görülene benzer X karşı iletkenliğinden bir davranışı gösterir, 2 .Orada&#39;da iletkenlikte bir ilk artışın ile x 1 ila 2 PAH oranı ve daha Li 1 TPB (THF) 24.7 için daha düşük bir Li ...

Lityum solvate elektron çözeltiler (LiSES) bu tür bifenil ve naftalen gibi basit iki halkalı poliaromatik hidrokarbonlar (PAH), potansiyel olarak Yakıt ikmali lityum hücreler 1-7 sıvı anot olarak kullanılabilir kullanılarak hazırlandı. LiSES, bu basit PAH moleküllerinin çözünmüş metalik lityum çözülmüş elektronların elektron reseptörleri olarak görev yaptı. Bu, iki halka sistemleri arasında ilerleyen yazarları, daha sonra daha karmaşık PAH&#39;ları kullanılarak siklopenta-2,4-dienon türevleri 8 grubundan başlayarak hazırlanır LiSES üzerine iletkenlik ölçme çalışmalar yapmışlardır yana. Bu PAH da aromatik halkalar dahil ikame edici ile büyük PAH (&gt; iki benzen halkası) ve PAH bulunmaktadır. İkiden fazla halkalı bir büyük PAH molekülü böylece daha yüksek bir enerji yoğunluğuna sahip LiSES elde bifenil ya da naftalin ya da daha PAH molekül başına lityum atomu yerleştirilmesi beklenmektedir. Girix amacıPAH içine ikame ediciler ing PAH daha kolay elektron kabul ve LiSES de polianyonlar olarak daha istikrarlı hale getirmek olduğunu. Yüksek enerji yoğunluğuna sahip LiSES geliştirmek için süregelen çabalarının bir parçası olarak, bu kağıt literatür prosedürüne 9 yanı sıra 1,3,5-triphenylbenzene tarafından yapılan corannulene hazırlanan LiSES karakterizasyonu hakkında rapor verecektir, TPB biraz değiştirilmiş literatürde 10 tarafından sentezlenen . Şekil 1 (1) &#39;de gösterildiği gibi 1,3,5-triphenylbenzene, iki ek fenil pozisyonlar 3 halkalar aynı halkanın 5 ile bir bifenil türevi olarak sınıflandırılabilir. bu molekül, dört benzen halkası olduğu için, daha bifenil daha molekül başına Li, 4 atomuna çekmesi gerekir ve naftalen (0.5 M çözelti, PAH başına Li maksimum 2.5 mol eşdeğer) (&lt;molekül başına lityumun 2.5 mol eşdeğer) . Corannulene Şekil 1 &#39;de gösterildiği gibi, PAH kase şekli halinde düzenlenmiş beş halkalı (2). Zabula ve ark., 11 corannulene iki kalıcı tetraanions arasına yerleştirilmiş beş Li + iyonları ile bir çözelti oluşturmak üzere corannulene / tetrahidrofuran (THF) içindeki bir çözeltisi içinde metalik lityum eritilmesi uygulanabilirliğini ortaya koymuştur. <img alt="Şekil 1" src="/files/ftp_upload/54366/54366fig1.jpg" /> Şekil 1:. 1,3,5-triphenylbenzene aynı halkanın konum 3 ve 5 de iki ilave fenil halkalı bir bifenil türevi olarak sınıflandırılır (1) ve corannulene (2) 1,3,5-triphenylbenzene moleküler yapıları . Corannulene bir kase şekline düzenlenmiş beş benzen halkaları ile beş halka PAH olduğunu. <a href="https://www.jove.com/files/ftp_upload/54366/54366fig1large.jpg" target="_blank">Bu rakamın büyük halini görmek için lütfen buraya tıklayınız.</a> Dolayısıyla, 1,3,5-triphenylbenzene ve corannulene hem de yüksek bir enerji için potansiyel adaylardıryoğunluk LiSES.

<table border="0" cellpadding="0" cellspacing="0" width="1005">
	<tbody>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Biphenyl Reagentplus, 99.5%</td>
			<td style="width:136px;">Sigma Aldrich</td>
			<td style="width:187px;">B34656-1KG</td>
			<td style="width:204px;"></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;">Tetrahydrofuran Anhydrous, 99.9%, Inhibi</td>
			<td style="width:136px;">Sigma Aldrich</td>
			<td>401757-100ML</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;">Iodine, Anhydrous, Beads, -10 Mesh, 99.999% trace metals basis&#160;</td>
			<td style="width:136px;">Sigma Aldrich</td>
			<td>451045-25G</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;">Lithium iodide, anhydrous, 99.95% (metals basis)</td>
			<td style="width:136px;">Alfa Aesar</td>
			<td>40666</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Lithium Ion Conducting Glass ceramics (Diameter 1&#34; x 150 mm)&#160;</td>
			<td style="width:136px;">Ohara</td>
			<td style="width:187px;">LICGC(AG01)</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Lithium Foil&#160;</td>
			<td style="width:136px;">Alfa Aesar</td>
			<td style="width:187px;">010769.14</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Methanol anhydrous, 99.8%</td>
			<td style="width:136px;">Sigma Aldrich</td>
			<td>322415-100ML&#160;</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">CompactStat : Electrochemical Analyser with Impedance</td>
			<td style="width:136px;">Ivium Technologies</td>
			<td style="width:187px;">Not Applicable</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Cond 3310 Conductivity Meter</td>
			<td style="width:136px;">WTW</td>
			<td style="width:187px;">Not Applicable</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:479px;">Digital Multimeter, Model Fluke 179</td>
			<td style="width:136px;">Fluke Corporation</td>
			<td style="width:187px;">Not Applicable</td>
			<td></td>
		</tr>
		<tr height="120">
			<td height="120" style="height:120px;width:479px;">1,3,5-triphenylbenzene</td>
			<td style="width:136px;">Synthesized from acetpohenone according to procedure described in literature</td>
			<td style="width:187px;"></td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Silicon tetrachloride</td>
			<td style="width:136px;">Sigma Aldrich</td>
			<td style="width:187px;">215120-100G</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">acetophenone</td>
			<td style="width:136px;">TCI</td>
			<td style="width:187px;">A0061-500g</td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:479px;">Ethanol</td>
			<td style="width:136px;">Merck Millipore</td>
			<td style="width:187px;">1.00983.2511</td>
			<td></td>
		</tr>
	</tbody>
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1,3,5-triphenylbenzene and corannulene as electron receptors for lithium solvated electron solutions

Yazarlar, lityum solvatlanmış elektron çözeltiler (LiSES) üzerinde gerçekleştirilen iletkenlik çalışmaları rapor elektron reseptör olarak, poliaromatik hidrokarbonlar iki tip (PAH), yani 1,3,5-triphenylbenzene ve corannulene kullanılarak hazırlandı. Katı PAH önce bir çözelti oluşturmak üzere, tetrahidrofuran (THF) içinde çözüldü. Metalik lityum daha sonra mavi veya yeşil, mavi çözeltiler, solvatlanmış elektronlar varlığının göstergesidir renge vermek üzere PAH / THF çözeltileri içinde çözülmüştür. Li ile ifade 1,3,5-triphenylbenzene tabanlı LiSES üzerinde gerçekleştirilmiştir, oda sıcaklığında, önceki iletkenlik ölçümleri TPB (THF) x 24.7 (x = 1, 2, 3, 4), Li artması ile iletkenlik bir artış gösterdi: X = 1&#39;den 2&#39;ye kadardır PAH oranı Ancak, iletkenlik giderek daha oranının artırılması sonra azalmıştır. Nitekim Li iletkenlik TPB (THF) x = 4 için 24.7 x daha düşüktür x </em&gt; = 1 Böyle bir davranış bifenil ve naftalinden hazırlanmıştır önce rapor LiSES ile verilene benzer. Li ile ifade corannulene tabanlı LiSES sıcaklık ölçümleri, karşılık iletkenlik Cor (THF) 247 (x = 1, 2, 3, 4, 5) gösterdi bifenil benzer bir metal davranışı gösteren negatif eğimli doğrusal ilişkiler ve naftalen-x tabanlı LiSES.

Şekil 2&#39;de gösterildiği gibi çeşitli lityum miktarları ve THF ile 1,3,5-triphenylbenzene karışımları arasındaki reaksiyon, yeşilimsi mavi veya koyu mavi renkli bir çözüm sunar. Bir açık renkli LiSES özel örneği solvatlanmış elektronlar düşük bir konsantrasyonuna sahip olduğunu gösterir. 0.5 M THF çözeltisi (Tablo 1) 1 ila 2 PAH oranı: 1,3,5-triphenylbenzene Li artması ile iletkenlik artışı göstermektedir. Bununla birlikte, iletkenlik değeri gidere...

Watch this Scientific Journal Video about 1,3,5-Triphenylbenzene and Corannulene as Electron Receptors for Lithium Solvated Electron Solutions at JoVE.com

1,3,5-Triphenylbenzene and Corannulene as Electron Receptors for Lithium Solvated Electron Solutions

The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using 1,3,5-triphenylbenzene (TPB) and corannulene as electron receptors.

Lityum Solvate Elektron Çözümleri Elektron Reseptör olarak 1,3,5-Triphenylbenzene ve Corannulene

The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using two types of polyaromatic ...

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Organic Chemistry

Chemistry

Unit 1

Reactions of Aromatic Compounds

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7.6K Görüntüleme.  Nanyang Technological University. The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using 1,3,5-triphenylbenzene (TPB) and corannulene as electron receptors.

Video: 1,3,5-Triphenylbenzene and Corannulene as Electron Receptors for Lithium Solvated Electron Solutions

Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples.

Trace explosive vapors of TNT and RDX collected on sorbent-filled thermal desorption tubes were analyzed using a programmed temperature desorption system coupled to GC with an electron capture detector. The instrumental analysis is combined with direct liquid deposition method to reduce sample variability and account for instrumentation drift and losses.

Programlı Sıcaklık Sızdırma Gaz Kromatografi-Elektron Yakalama Dedektörü tarafından Trace Patlayıcı Buharlar Nicel Saptanması

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive ...

Kimya

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

Muntazam olmayan biçimde Pr-katkılı SrTiO sentezi<sub&gt; 3</sub&gt; Seramik ve Bunların termoelektrik Özellikleri

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma ...

Characterizing Electron Transport through Living Biofilms

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under physiologically relevant conditions.1 These measurements are performed on living biofilms in aqueous medium using source and drain electrodes patterned on a glass surface in a specialized configuration referred to as an interdigitated electrode (IDA) array. A biofilm is grown that extends across the gap connecting the source and drain. Potentials are applied to the electrodes (ES and ED) generating a source-drain current (ISD) through the biofilm between the electrodes. The dependency of electrical conductivity on gate potential (the average of the source and drain potentials, EG = [ED + ES]/2) is determined by systematically changing the gate potential and measuring the resulting source-drain current. The dependency of conductivity on gate potential provides mechanistic information about the extracellular electron transport process underlying the electrical conductivity of the specific biofilm under investigation. The electrochemical gating measurement method described here is based directly on that used by M. S. Wrighton2,3 and colleagues and R. W. Murray4,5,6 and colleagues in the 1980&#39;s to investigate thin film conductive polymers.

A protocol for measuring electrical conductivity of living microbial biofilms under physiologically relevant conditions is presented.

Elektron taşıma yaşayan biyofilmler ile karakterize

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

Geliştirilmiş Elektron İletken özellikleri ile Fe-katkılı Alüminosilikat Nanotüpler Sentezi ve Karakterizasyonu

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully understood. We have traced the trajectories of individual nanoparticles using liquid-cell transmission electron microscopy (TEM) to investigate the mechanism of the assembly process. Herein, we present the protocols used for liquid-cell TEM studies of the self-assembly mechanism. First, we introduce the detailed synthetic protocols used to produce uniformly sized platinum and lead selenide nanoparticles. Next, we present the microfabrication processes used to produce liquid cells with silicon nitride or silicon windows and then describe the loading and imaging procedures of the liquid-cell TEM technique. Several notes are included to provide helpful tips for the entire process, including how to manage the fragile cell windows. The individual motions of nanoparticles tracked by liquid-cell TEM revealed that changes in the solvent boundaries caused by evaporation affected the self-assembly process of nanoparticles. The solvent boundaries drove nanoparticles to primarily form amorphous aggregates, followed by flattening of the aggregates to produce a 2-dimensional (2D) self-assembled structure. These behaviors are also observed for different nanoparticle types and different liquid-cell compositions.

Here we introduce experimental protocols for the real-time observation of a self-assembly process using liquid-cell transmission electron microscopy.

Hücre içi sıvı iletim elektron mikroskobu nano tanecikleri, kendinden montajlı takibi için

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography

Energy filtered transmission electron microscopy tomography (EFTEM tomography) can provide three-dimensional (3D) chemical maps of materials at a nanometric scale. EFTEM tomography can separate chemical elements that are very difficult to distinguish using other imaging techniques. The experimental protocol described here shows how to create 3D chemical maps to understand the chemical distribution and morphology of a material. Sample preparation steps for data segmentation are presented. This protocol permits the 3D distribution analysis of chemical elements in a nanometric sample. However, it should be noted that currently, the 3D chemical maps can only be generated for samples that are not beam sensitive, since the recording of filtered images requires long exposure times to an intense electron beam. The protocol was applied to quantify the chemical distribution of the components of two different heterogeneous catalyst supports. In the first study, the chemical distribution of aluminum and titanium in titania-alumina supports was analyzed. The samples were prepared using the swing-pH method. In the second, the chemical distribution of aluminum and silicon in silica-alumina supports that were prepared using the sol-powder and mechanical mixture methods was examined.

This paper describes a protocol to achieve 3D chemical maps combining energy filtered imaging and electron tomography. The chemical distribution of two catalyst supports formed by elements that are difficult to distinguish by other imaging techniques was studied. Each application consists of mapping overlapped chemical elements - respectively spaced-ionization edges.

3D kimyasal haritalar tarafından enerji elde etme transmisyon elektron mikroskobu tomografi filtre

Energy filtered transmission electron microscopy tomography (EFTEM tomography) can provide three-dimensional (3D) chemical maps of materials at a ...

An Experimental Protocol for Femtosecond NIR/UV - XUV Pump-Probe Experiments with Free-Electron Lasers

This protocol describes key steps in performing and analyzing femtosecond pump-probe experiments that combine a femtosecond optical laser with a free-electron laser. This includes methods to establish the spatial and temporal overlap between the optical and free-electron laser pulses during the experiment, as well as important aspects of the data analysis, such as corrections for arrival time jitter, which are necessary to obtain high-quality pump-probe data sets with the best possible temporal resolution. These methods are demonstrated for an exemplary experiment performed at the FLASH (Free-electron LASer Hamburg) free-electron laser in order to study ultrafast photochemistry in gas-phase molecules by means of velocity map ion imaging. However, most of the strategies are also applicable to similar pump-probe experiments using other targets or other experimental techniques.

This protocol describes the key steps for performing and analyzing pump-probe experiments combining a femtosecond optical laser with a free-electron laser in order to study ultrafast photochemical reactions in gas-phase molecules.

Bir deneysel protokol için Femtosecond NIR/UV-serbest elektron lazerler ile XUV pompa-sonda deneyler

This protocol describes key steps in performing and analyzing femtosecond pump-probe experiments that combine a femtosecond optical laser with a ...

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 &#181;m grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes in detail how to fabricate and operate microfluidic devices for X-ray diffraction data collection at room temperature. Additionally, it describes how to monitor protein crystallization by dynamic light scattering and how to process and analyze obtained diffraction data.

Mikrosıvısal çip Situ Crystal x-ışını kırınım ve in Situ dinamik ışık saçılma seri kristalografisi için için

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various precursor noble metal ions with reducing agents in a 1:1 (v/v) ratio results in the formation of metal gels within seconds to minutes compared to much longer synthesis times for other techniques such as sol-gel. Conducting the reduction step in a microcentrifuge tube or small volume conical tube facilitates a proposed nucleation, growth, densification, fusion, equilibration model for gel formation, with final gel geometry smaller than the initial reaction volume. This method takes advantage of the vigorous hydrogen gas evolution as a by-product of the reduction step, and as a consequence of reagent concentrations. The solvent accessible specific surface area is determined with both electrochemical impedance spectroscopy and cyclic voltammetry. After rinsing and freeze drying, the resulting aerogel structure is examined with scanning electron microscopy, X-ray diffractometry, and nitrogen gas adsorption. The synthesis method and characterization techniques result in a close correspondence of aerogel ligament sizes. This synthesis method for noble metal aerogels demonstrates that high specific surface area monoliths may be achieved with a rapid and direct reduction approach.

A rapid, direct solution-based reduction synthesis method to obtain Au, Pd, and Pt aerogels is presented.

Otomatik Güncelleştirmeler, Pd ve Pt Aerogels üzerinden doğrudan çözüm tabanlı azaltma için hızlı sentez yöntemi

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Pretargeted Radioimmunotherapy Based on the Inverse Electron Demand Diels-Alder Reaction

While radioimmunotherapy (RIT) is a promising approach for the treatment of cancer, the long pharmacokinetic half-life of radiolabeled antibodies can result in high radiation doses to healthy tissues. Perhaps not surprisingly, several different strategies have been developed to circumvent this troubling limitation. One of the most promising of these approaches is pretargeted radioimmunotherapy (PRIT). PRIT is predicated on decoupling the radionuclide from the immunoglobulin, injecting them separately, and then allowing them to combine in vivo at the target tissue. This approach harnesses the exceptional tumor-targeting properties of antibodies while skirting their pharmacokinetic drawbacks, thereby lowering radiation doses to non-target tissues and facilitating the use of radionuclides with half-lives that are considered too short for use in traditional radioimmunoconjugates. Over the last five years, our laboratory and others have developed an approach to in vivo pretargeting based on the inverse electron-demand Diels-Alder (IEDDA) reaction between trans-cyclooctene (TCO) and tetrazine (Tz). This strategy has been successfully applied to pretargeted positron emission tomography (PET) and single-photon emission computed tomography (SPECT) imaging with a variety of antibody-antigen systems. In a pair of recent publications, we have demonstrated the efficacy of IEDDA-based PRIT in murine models of pancreatic ductal adenocarcinoma and colorectal carcinoma. In this protocol, we describe protocols for PRIT using a 177Lu-DOTA-labeled tetrazine radioligand ([177Lu]Lu-DOTA-PEG7-Tz) and a TCO-modified variant of the colorectal cancer targeting huA33 antibody (huA33-TCO). More specifically, we will describe the construction of huA33-TCO, the synthesis and radiolabeling of [177Lu]Lu-DOTA-PEG7-Tz, and the performance of in vivo biodistribution and longitudinal therapy studies in murine models of colorectal carcinoma.

This protocol describes the synthesis and characterization of a trans-cyclooctene (TCO)-modified antibody and a 177Lu-labeled tetrazine (Tz) radioligand for pretargeted radioimmunotherapy (PRIT). In addition, it details the use of these two constructs for in vivo biodistribution and longitudinal therapy studies in a murine model of colorectal cancer.

Pretargeted Radioimmunotherapy ters elektron talep Diels-Alder reaksiyonu üzerinde dayalı

While radioimmunotherapy (RIT) is a promising approach for the treatment of cancer, the long pharmacokinetic half-life of radiolabeled antibodies can ...