著者らは、Rutgers大学のThomas J. Emge博士とWei Liu博士に、小角X線回折と粉末X線回折の分析と専門知識について高く評価しています。さらに、著者らは、N 2吸着実験でのHao Wangの支持について認めている。

1.Al（OH） 3ナノ粒子合成<ol><li> 1.40gの塩化アルミニウム六水和物を5.822gの脱イオン水に溶解する。 </li><li>磁気撹拌しながら、2.778gのL-アルギニンを塩化アルミニウム水溶液に添加する。添加されたアルギニンが溶解し、大きな塊または塊を形成しないように、L-アルギニンをゆっくりと添加する。さらに、ゆっくりと添加すると、局所的なアルカリ濃度が低下し、より制御しやすい加水分解のための条件が提供される。 </li><li>すべてのアルギニンが溶液に溶解したら、溶液を50℃で72時間加熱します。この時点で、ソリューションは曇ったサスペンションとして表示されることがあります。 </li></ol> 2.Al（OH） 3をNaClで析出させる<ol><li>直径49インチ、長さ1.125のGPCカラムを準備する。ゲルを添加し、水をカラムに通して適切な充填を確実にするために、ゲルビーズ間の空間を最小限にして、ゲルを連続的にパックする。パックゲルからカラムの約80％まで;パックされたゲルの量は毎回変化し、分離した種の保持時間にのみ影響する。 </li><li> 10mL注入器ループを備えたHPLCポンプを用いて、10mLの合成されたままのAl（OH） 3ナノ粒子懸濁液（ステップ1.3で調製）をカラムに導入する。チューブの外径が約0.125インチで、注入されたサンプルを10mL送達するように校正されたチューブを使用してインジェクタループをカスタム化します。 </li><li> dRIのピーク位置に相関する間隔でカラム溶出を収集する。 GPC出力を示差屈折率（dRI）検出器の入力に接続します。 注：分離された種はGPCから出てくるので、ピークとしてdRI検出器に現れ、その後125mLボトルに集められます。 GPCカラムは、2つのよく分離されたピークを生成し、それらは両方とも集められ、サイズ排除クロマトグラフィー（SEC）および元素分析（EA）によって分析され、アルギニンをアルミニウムスピンから区別するcies。収集される全容積は、GPCカラムのサイズ、使用される充填材料の総量、およびカラムを溶出するために使用される脱イオン水の流速に依存する。 <ol><li> 0.2mL /分の流速で100分かけてピーク1画分の大部分を集める。 </li><li> GPCカラムのRI検出器にピークが現れたら、30分間隔で溶離液を集める。 注：間隔の範囲を変更すると、結果として得られる精製されたピーク1物質の濃度と純度が変わります。最初にピークの小さな間隔を収集して、特定のカラムについてピーク1種の最高濃度と純度を含む部分を決定する方が良いです。 </li></ol></li><li> 1重量％のNaClを調製する。 </li><li>調製したNaCl溶液を10mLの精製Al（OH） 3ナノ粒子に滴下して加える。 NaCl沈殿を用いて調製した材料は、さらなる実験に使用しない。 </li></ol> Al-MCM-41の調製<ol><li> Ac約1.0gのMCM-41を真空オーブン中で120℃、3時間真空下で揺動させる。 </li><li> 9.6926gのAlCl 3・6H 2 Oを40.3074gの脱イオン水と混合することにより50.0gの塩化アルミニウム溶液を調製する。 </li><li> 0.7gの活性化MCM-41を50.0gの塩化アルミニウム溶液（工程3.2で調製）に加える。 </li><li> MCM-41チャンネル全体に拡散したAlCl 3の均質性を確実にするために、適切な混合時間（1時間）を与えます。 </li><li>磁気撹拌下で、L-アルギニンを2.75のArg / Alモル比に異種混合物に添加する。工程1.2と同様に、瞬時に形成された凝集物を再溶解させ、添加を続ける前にアルギニンの凝集を減少させるのに十分なほどゆっくりとアルギニンを添加する。 </li><li>均質になったら、混合物を50℃で72時間加熱する。 </li><li>得られた不均質溶液をブフナー漏斗を用いて真空下で濾過し、定性的な90mm濾紙円（または任意の他の適切なろ紙）。 </li><li>ろ過した白色粉末を過剰の脱イオン水で洗浄して、生成したAl-MCM-41材料から未反応の塩化アルミニウム、アルギニンまたは水溶性副生成物を確実に除去する。 </li></ol>

<ol>
	<li>Laden, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Antiperspirants and Deodorants. , (1999).</li><li>Kumara, C. K., Ng, W. J., Bandara, A., Weerasooriya, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanogibbsite:+Synthesis+and+characterization.">Nanogibbsite: Synthesis and characterization.</a> J. Colloid Interface Sci. 352 (2), 252-258 (2010).</li><li>Demichelis, R., Noel, Y., Ugliengo, P., Zicovich-Wilson, C. M., Dovesi, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physico-Chemical+Features+of+Aluminum+Hydroxides+As+Modeled+with+the+Hybrid+B3LYP+Functional+and+Localized+Basis+Functions.">Physico-Chemical Features of Aluminum Hydroxides As Modeled with the Hybrid B3LYP Functional and Localized Basis Functions.</a> J.Phys. Chem. C. 115 (27), 13107-13134 (2011).</li><li>Elderfield, H., Hem, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+development+of+crystalline+structure+in+aluminum+hydroxide+polymorphs+on+ageing.">The development of crystalline structure in aluminum hydroxide polymorphs on ageing.</a> Mineral. Mag. 39, 89-96 (1973).</li><li>Wang, S. L., Johnston, C. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Assignment+of+the+structural+OH+stretching+bands+of+gibbsite.">Assignment of the structural OH stretching bands of gibbsite.</a> Am. Mineral. 85, 739-744 (2000).</li><li>Balan, E., Lazzer, M., Morin, G., Mauri, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=First-principles+study+of+the+OH-stretching+modes+of+gibbsite.">First-principles study of the OH-stretching modes of gibbsite.</a> Am. Mineral. 91 (1), 115-119 (2006).</li><li>Scherrer, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bestimmung+der+Grosse+und+der+inneren+Struktur+von+Kolloidteilchen+mittels+Rontgenstrahlen+.">Bestimmung der Grosse und der inneren Struktur von Kolloidteilchen mittels Rontgenstrahlen .</a> Gottingen. 26, 98-100 (1918).</li><li>Langford, J. I., Wilson, A. J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Scherrer+after+sixty+years:+a+survey+and+some+new+results+in+the+determination+of+crystallite+size.">Scherrer after sixty years: a survey and some new results in the determination of crystallite size.</a> J. Appl. Cryst. 11 (2), 102-113 (1978).</li><li>Swaddle, T. W., 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=Kinetic+Evidence+for+Five-Coordination+in+AlOH(aq)2++Ion.">Kinetic Evidence for Five-Coordination in AlOH(aq)2+ Ion.</a> Science. 308 (5727), 1450-1453 (2005).</li><li>Casey, W. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large+Aqueous+Aluminum+Hydroxide+Molecules.">Large Aqueous Aluminum Hydroxide Molecules.</a> Chem. Rev. 106 (1), 1-16 (2006).</li><li>Lutzenkirchen, J., 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=Adsorption+of+Al13-Keggin+clusters+to+sapphire+c-plane+single+crystals:+Kinetic+observations+by+streaming+current+measurements.">Adsorption of Al13-Keggin clusters to sapphire c-plane single crystals: Kinetic observations by streaming current measurements.</a> Appl. Surf. Sci. 256 (17), 5406-5411 (2010).</li><li>Mokaya, R., Jones, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Efficient+post-synthesis+alumination+of+MCM-41+using+aluminum+chlorohydrate+containing+Al+polycations.">Efficient post-synthesis alumination of MCM-41 using aluminum chlorohydrate containing Al polycations.</a> J. Mater. Chem. 9 (2), 555-561 (1999).</li><li>Brunauer, S., Deming, L. S., Deming, W. E., Teller, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On+a+Theory+of+the+van+der+Waals+adsorption+of+gases.">On a Theory of the van der Waals adsorption of gases.</a> J. Am. Chem. Soc. 62 (7), 1723-1732 (1940).</li><li>Kresge, C. T., Leonowicz, M. E., Roth, W. J., Vartuli, J. C., Beck, 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=Ordered+mesoporous+molecular+sieves+synthesized+by+a+liquid-crystal+template+mechanism.">Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism.</a> Nature. 359 (6397), 710-712 (1992).</li><li>Zeng, Q., Nekvasil, H., Grey, C. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Proton+Environments+in+Hydrous+Aluminosilicate+Glasses:+A+1H+MAS,+1H/27Al,+and+1H/23Na+TRAPDOR+NMR+Study.">Proton Environments in Hydrous Aluminosilicate Glasses: A 1H MAS, 1H/27Al, and 1H/23Na TRAPDOR NMR Study.</a> J. Phys. Chem. B. 103 (35), 7406-7415 (1999).</li><li>Kao, H. M., Grey, C. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Probing+the+Bronsted+and+Lewis+acidity+of+zeolite+HY:+A+1H/27Al+and+15N/27Al+TRAPDOOR+NMR+study+of+mono-methylamine+adsorbed+on+HY.">Probing the Bronsted and Lewis acidity of zeolite HY: A 1H/27Al and 15N/27Al TRAPDOOR NMR study of mono-methylamine adsorbed on HY.</a> J. Phys. Chem. 100 (12), 5105-5117 (1996).</li><li>DeCanio, E. C., Edwards, J. C., Bruno, J. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid-state+1H+MAS+NMR+characterization+of+&#947;-alumina+and+modified+&#947;-aluminas.">Solid-state 1H MAS NMR characterization of &#947;-alumina and modified &#947;-aluminas.</a> J. Catal. 148 (1), 76-83 (1994).</li><li>Shafran, K. L., Deschaume, O., Perry, C. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+static+anion+exchange+method+for+generation+of+high+purity+aluminium+polyoxocations+and+monodisperse+aluminum+hydroxide+nanoparticles.">The static anion exchange method for generation of high purity aluminium polyoxocations and monodisperse aluminum hydroxide nanoparticles.</a> J. Mater. Chem. 15 (33), 3415-3423 (2005).</li><li>Vogels, R. J. M. J., Kloprogge, J. T., Geus, J. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Homogeneous+forced+hydrolysis+of+aluminum+through+the+thermal+decomposition+of+urea.">Homogeneous forced hydrolysis of aluminum through the thermal decomposition of urea.</a> J. Colloid Interface Sci. 285 (1), 86-93 (2005).</li></ol>

著者は何も開示することはない。

塩化アルミニウム水溶液の調製には、塩化アルミニウムの結晶六水和物塩の使用が必要であった。無水形態も使用することができるが、重要な吸湿特性のために好ましくない。そのため、アルミニウムの濃度を制御したり、アルミニウムの濃度を制御することが困難になる。時間の経過とともに、[Al（H 2 O） 6 ] 3+アクア酸が加水分解して最終的に全体の収率および最?...

水酸化アルミニウムで作られた材料は、触媒、医薬品、水処理、化粧品を含む様々な産業用途の有望な候補である。 1,2,3,4 高温では、水酸化アルミニウムは分解中に相当量の熱を吸収してアルミナ（Al 2 O 3 ）を生成し、それを有用な難燃剤にする。水酸化アルミニウムの4つの既知の多形体（ すなわち 、ギブサイト、バイエライト、ノードストランダイト、およびドイライト）は、それらの形成および構造に関する我々の理解を改善するために、計算および実験技術を用いて研究されている6 。ナノスケールの粒子の調製は、量子効果およびそれらの特性とは異なる特性を示す可能性があるため、特に重要であるrバルクカウンターパート。 100nmのオーダの寸法を有するナノギブサイト粒子は、様々な条件7,8,9,10,11,12,13,14で容易に調製される。 粒径をさらに小さくすることに伴う固有の課題を克服することはさらに困難である。したがって、ナノギブサイト粒子が50nm程度の寸法を有する場合はごくわずかである。私たちの知る限りでは、50nmより小さいナノギブサイトの報告はありませんでした。部分的には、これは、ナノ粒子が静電的不安定性のために凝集する傾向があるという事実に起因するコロイド粒子間、特に極性プロトン性溶媒中での水素結合の形成の可能性が高い。私たちの目的は、安全な成分と前駆物質だけを使って小さなAl（OH） 3ナノ粒子を合成することでした。現在の研究では、緩衝液および安定剤としてアミノ酸（ すなわち 、L-アルギニン）を組み込むことによって、水性粒子凝集が阻害された。さらに、グアニジニウム含有アルギニンは水酸化アルミニウム粒子の成長および凝集を防止し、平均粒径が10〜30nmのコロイド懸濁液を生成することが報告されている。ここでアルギニンの両性および双性イオン性の性質は、30nmを超える粒子成長を不快にする穏やかな加水分解の間に水酸化アルミニウムナノ粒子の表面電荷を緩和することが提案されている。アルギニンは10nm未満の粒子サイズを減少させることができなかったが、このような粒子は、「ケージ」閉じ込め効果を利用して達成されたMCM-41のメソ細孔内に存在する。 Al-MCM-41複合材料のキャラクタリゼーションは、平均孔径2.7nmを有するメソポーラスシリカ内の超微細水酸化アルミニウムナノ粒子を明らかにした。

<table border="0" cellpadding="0" cellspacing="0" width="650">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:261px;">aluminum chloride hexahydrate</td>
			<td style="width:103px;">Alfa Aesar</td>
			<td align="right" style="width:119px;">12297</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:261px;">L-arginine</td>
			<td style="width:103px;">BioKyowa</td>
			<td style="width:119px;">N/A</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:261px;">aluminum hydroxide</td>
			<td style="width:103px;">Sigma Aldrich</td>
			<td align="right" style="width:119px;">239186</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:261px;">Bio-Gel P-4 Gel</td>
			<td style="width:103px;">Bio-Rad</td>
			<td style="width:119px;">150-4128</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:261px;">Mesoporous siica (MCM-41 type)</td>
			<td style="width:103px;">Sigma Aldrich</td>
			<td align="right" style="width:119px;">643645</td>
			<td></td>
		</tr>
	</tbody>
</table>

facile preparation of ultrafine aluminum hydroxide particles with or without mesoporous mcm-41 in ambient environments

ナノギブサイトの水性懸濁液を、L-アルギニンとpH6.6のアルミニウムアクア酸[Al（H 2 O） 6 ] 3+の滴定によって合成した。水性アルミニウム塩の加水分解は広範囲のサイズ分布を有する幅広い製品を生成することが知られているので、種々の最先端装置（ すなわち 27 Al / 1 H NMR、FTIR、ICP-OES 、TEM-EDX、XPS、XRD、およびBET）を使用して、合成生成物および副産物の同定を特徴付けた。ゲル透過クロマトグラフィー（GPC）カラム技術を用いてナノ粒子（10〜30nm）からなる生成物を単離した。フーリエ変換赤外（FTIR）分光法および粉末X線回折（PXRD）は、精製材料を水酸化アルミニウムのギブサイト多形体であると同定した。無機塩（ 例えば 、NaCl）の添加は、懸濁液の静電的不安定化を誘導し、それによってナノ粒子を凝集させて大粒径のAl（OH） 3沈殿物。本明細書に記載の新規な合成方法を利用することにより、Al（OH） 3は、MCM-41の高度に秩序化されたメソポーラス骨格内部に部分的に充填され、平均孔寸法は2.7nmであり、八面体および四面体Al（Oh / T d = 1.4）。エネルギー分散型X線分光分析（EDX）を用いて測定した総Al含有量は11％w / wであり、Si / Alモル比は2.9であった。バルクEDXと表面X線光電子分光法（XPS）元素分析とを比較することにより、アルミノケイ酸塩材料内のAlの分布についての洞察が得られた。さらに、バルク（2.9）と比較して、Si / Alの高い比が外部表面（3.6）で観察された。 O / Al比の近似は、それぞれコアおよび外部表面近くのAl（O） 3およびAl（O） 4基のより高い濃度を示唆している。新たに開発されたAl-MCM-41の合成は、Al 2 O 3ナノ粒子が有利である用途に使用することができる。

Nanogibbsite Synthesis ナノギブサイトは、AlCl 3・6H 2 O（14重量％）をL-アルギニンで滴定し、最終Arg / Alモル比が2.75になるように調製した。ナノギブサイト粒子の合成は、部分的に加水分解された塩化アルミニウム溶液のために広く使用されている分析技術であるSECを介してモニターされ、ピーク1,2,3,4およ...

Watch this Scientific Journal Video about Facile Preparation of Ultrafine Aluminum Hydroxide Particles with or without Mesoporous MCM-41 in Ambient Environments at JoVE.com

Facile Preparation of Ultrafine Aluminum Hydroxide Particles with or without Mesoporous MCM-41 in Ambient Environments

超微細水酸化アルミニウムナノ粒子懸濁液を、MCM-41のメソポーラスチャンネル内にケージ効果閉じ込めを伴うかまたは伴わないで、L-アルギニンを用いた[Al（H 2 O）] 3+の pHを4.6に制御滴定することによって調製した。

周囲環境におけるメソ多孔性MCM-41を有するまたは含まない超微粒水酸化アルミニウム粒子の容易な調製

An aqueous suspension of nanogibbsite was synthesized via the titration of aluminum aqua acid [Al(H2O)6]3+ with L-arginine to pH 4.6. Since the hydrolysis ...

facile-preparation-ultrafine-aluminum-hydroxide-particles-with-or

Research

JoVE Journal

Chemistry

10.8K ビュー.  Colgate-Palmolive Company. 超微細水酸化アルミニウムナノ粒子懸濁液を、MCM-41のメソポーラスチャンネル内にケージ効果閉じ込めを伴うかまたは伴わないで、L-アルギニンを用いた[Al（H 2 O）] 3+の pHを4.6に制御滴定することによって調製した。 

ビデオ: Facile Preparation of Ultrafine Aluminum Hydroxide Particles with or without Mesoporous MCM-41 in Ambient Environments

Particles without a Box: Brush-first Synthesis of Photodegradable PEG Star Polymers under Ambient Conditions

Convenient methods for the rapid, parallel synthesis of diversely functionalized nanoparticles will enable discovery of novel formulations for drug delivery, biological imaging, and supported catalysis. In this report, we demonstrate parallel synthesis of brush-arm star polymer (BASP) nanoparticles by the &#34;brush-first&#34; method. In this method, a norbornene-terminated poly(ethylene glycol) (PEG) macromonomer (PEG-MM) is first polymerized via ring-opening metathesis polymerization (ROMP) to generate a living brush macroinitiator. Aliquots of this initiator stock solution are added to vials that contain varied amounts of a photodegradable bis-norbornene crosslinker. Exposure to crosslinker initiates a series of kinetically-controlled brush+brush and star+star coupling reactions that ultimately yields BASPs with cores comprised of the crosslinker and coronas comprised of PEG. The final BASP size depends on the amount of crosslinker added. We carry out the synthesis of three BASPs on the benchtop with no special precautions to remove air and moisture. The samples are characterized by gel permeation chromatography (GPC); results agreed closely with our previous report that utilized inert (glovebox) conditions. Key practical features, advantages, and potential disadvantages of the brush-first method are discussed.

Poly(ethylene glycol) (PEG) brush-arm star polymers (BASPs) with narrow mass distributions and tunable nanoscopic sizes are synthesized in via ring opening metathesis polymerization (ROMP) of a PEG-norbornene macromonomer followed by transfer of portions of the resulting living brush initiator to vials containing varied amounts of a rigid, photo-cleavable bis-norbornene crosslinker.

周囲条件下での光分解性のPEGスターポリマーのブラシ、最初の合成：箱なしの粒子

Convenient methods for the rapid, parallel synthesis of diversely functionalized nanoparticles will enable discovery of novel formulations for drug ...

化学

Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic cavitation: the nucleation, growth, and implosive collapse of microbubbles in liquids submitted to power ultrasound. The violent implosion of bubbles leads to the formation of chemically reactive species and to the emission of light, named sonoluminescence. In this manuscript, we describe the techniques allowing study of extreme intrabubble conditions and chemical reactivity of acoustic cavitation in solutions. The analysis of sonoluminescence spectra of water sparged with noble gases provides evidence for nonequilibrium plasma formation. The photons and the "hot" particles generated by cavitation bubbles enable to excite the non-volatile species in solutions increasing their chemical reactivity. For example the mechanism of ultrabright sonoluminescence of uranyl ions in acidic solutions varies with uranium concentration: sonophotoluminescence dominates in diluted solutions, and collisional excitation contributes at higher uranium concentration. Secondary sonochemical products may arise from chemically active species that are formed inside the bubble, but then diffuse into the liquid phase and react with solution precursors to form a variety of products. For instance, the sonochemical reduction of Pt(IV) in pure water provides an innovative synthetic route for monodispersed nanoparticles of metallic platinum without any templates or capping agents. Many studies reveal the advantages of ultrasound to activate the divided solids. In general, the mechanical effects of ultrasound strongly contribute in heterogeneous systems in addition to chemical effects. In particular, the sonolysis of PuO2 powder in pure water yields stable colloids of plutonium due to both effects.

Acoustic cavitation in liquids submitted to power ultrasound creates transient extreme conditions inside the collapsing bubbles, which are the origin of unusual chemical reactivity and light emission, known as sonoluminescence. In the presence of noble gases, nonequilibrium plasma is formed. The "hot" particles and the photons generated by collapsing bubbles are able to excite species in solution.

分子、イオン、および音響キャビテーションと固体粒子を活性化

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic ...

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

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties of the materials were investigated. We used a one pot sol-gel approach to intercalate gold nano particles in the walls of mesoporous silica. To start with the synthesis, P123 was used as template to form micelles. Then TESPTS was used as a surface modification agent to intercalate gold nano particles. Following this process, TEOS was added in as a silica source which underwent a polymerization process in acid environment. After hydrothermal processing and calcination, the final product was acquired. Several techniques were utilized to characterize the porosity, morphology and structure of the gold intercalated mesoporous silica. The results showed a stable structure of mesoporous silica after gold intercalation. Through the oxidation of benzyl alcohol as a benchmark reaction, the GMS materials showed high selectivity and recyclability.

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.

合成とメソポーラスシリカの壁に金インターカレーの触媒性能

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

Facile and Efficient Preparation of Tri-component Fluorescent Glycopolymers via RAFT-controlled Polymerization

Synthetic glycopolymers are instrumental and versatile tools used in various biochemical and biomedical research fields. An example of a facile and efficient synthesis of well-controlled fluorescent statistical glycopolymers using reversible addition-fragmentation chain-transfer (RAFT)-based polymerization is demonstrated. The synthesis starts with the preparation of &#946;-galactose-containing glycomonomer 2-lactobionamidoethyl methacrylamide obtained by reaction of lactobionolactone and N-(2-aminoethyl) methacrylamide (AEMA). 2-Gluconamidoethyl methacrylamide (GAEMA) is used as a structural analog lacking a terminal &#946;-galactoside. The following RAFT-mediated copolymerization reaction involves three different monomers: N-(2-hydroxyethyl) acrylamide as spacer, AEMA as target for further fluorescence labeling, and the glycomonomers. Tolerant of aqueous systems, the RAFT agent used in the reaction is (4-cyanopentanoic acid)-4-dithiobenzoate. Low dispersities (&#8804;1.32), predictable copolymer compositions, and high reproducibility of the polymerizations were observed among the products. Fluorescent polymers are obtained by modifying the glycopolymers with carboxyfluorescein succinimidyl ester targeting the primary amine functional groups on AEMA. Lectin-binding specificities of the resulting glycopolymers are verified by testing with corresponding agarose beads coated with specific glycoepitope recognizing lectins. Because of the ease of the synthesis, the tight control of the product compositions and the good reproducibility of the reaction, this protocol can be translated towards preparation of other RAFT-based glycopolymers with specific structures and compositions, as desired.

An efficient, three-step synthesis of RAFT-based fluorescent glycopolymers, consisting of glycomonomer preparation, copolymerization, and post-modification, is demonstrated. This protocol can be used to prepare RAFT-based statistical glycopolymers with desired structures.

RAFT制御重合によるトライ成分蛍光グリコの容易かつ効率的な準備

Synthetic glycopolymers are instrumental and versatile tools used in various biochemical and biomedical research fields. An example of a facile and ...

Construction and Systematical Symmetric Studies of a Series of Supramolecular Clusters with Binary or Ternary Ammonium Triphenylacetates

Functions of clusters in nano or sub-nano scale significantly depend on not only kinds of their components but also arrangements, or symmetry, of their components. Therefore, the arrangements in the clusters have been precisely characterized, especially for metal complexes. Contrary to this, characterizations of molecular arrangements in supramolecular clusters composed of organic molecules are limited to a few cases. This is because construction of the supramolecular clusters, especially obtaining a series of the supramolecular clusters, is difficult due to low stability of non-covalent bonds compare to covalent bonds. From this viewpoint, utilization of organic salts is one of the most useful strategies. A series of the supramolecules could be constructed by combinations of a specific organic molecule with various counter ions. Especially, primary ammonium carboxylates are suitable as typical examples of supramolecules because various kinds of carboxylic acids and primary amines are commercially available, and it is easy to change their combinations. Previously, it was demonstrated that primary ammonium triphenylacetates using various kinds of primary amines specifically construct supramolecular clusters, which are composed of four ammoniums and four triphenylacetates assembled by charge-assisted hydrogen bonds, in crystals obtained from non-polar solvents. This study demonstrates an application of the specific construction of the supramolecular clusters as a strategy to conduct systematical symmetric study for clarification of correlations between molecular arrangements in supramolecules and kinds and numbers of their components. In the same way with binary salts composed of triphenylacetates and one kind of primary ammoniums, ternary organic salts composed of triphenylacetates and two kinds of ammoniums construct the supramolecular clusters, affording a series of the supramolecular clusters with various kinds and numbers of the components.

This article describes construction of a series of hydrogen-bonding supramolecular clusters in crystals using primary ammonium triphenylacetates, which are recrystallized from non-polar solvents. This selective construction of the supramolecular clusters leads to effective systematical symmetric studies about a correlation between the supramolecular clusters and their components.

バイナリまたは三元アンモニウムTriphenylacetatesと超分子クラスターのシリーズの構築と体系的対称研究

Functions of clusters in nano or sub-nano scale significantly depend on not only kinds of their components but also arrangements, or symmetry, of their ...

Facile Preparation of Internally Self-assembled Lipid Particles Stabilized by Carbon Nanotubes

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled (functionalized) CNTs are used as stabilizers to produce Pickering type oil-in-water (O/W) emulsions. Lipids namely, Dimodan U and Phytantriol are used as emulsifiers, which in excess water self-assemble into the bicontinuous cubic Pn3m phase. This highly viscous phase is fragmented into smaller particles using a probe ultrasonicator in presence of conventional surfactant stabilizers or CNTs as done here. Initially, the CNTs (powder form) are dispersed in water followed by further ultrasonication with the molten lipid to form the final emulsion. During this process the CNTs get coated with lipid molecules, which in turn are presumed to surround the lipid droplets to form a particulate emulsion that is stable for months. The average size of CNT-stabilized nanostructured lipid particles is in the submicron range, which compares well with the particles stabilized using conventional surfactants. Small angle X-ray scattering data confirms the retention of the original Pn3m cubic phase in the CNT-stabilized lipid dispersions as compared to the pure lipid phase (bulk state). Blue shift and lowering of the intensities in characteristic G and G&#39; bands of CNTs observed in Raman spectroscopy characterize the interaction between CNT surface and lipid molecules. These results suggest that the interactions between the CNTs and lipids are responsible for their mutual stabilization in aqueous solutions. As the concentrations of CNTs employed for stabilization are very low and lipid molecules are able to functionalize the CNTs, the toxicity of CNTs is expected to be insignificant while their biocompatibility is greatly enhanced. Hence the present approach finds a great potential in various biomedical applications, for instance, for developing hybrid nanocarrier systems for the delivery of multiple functional molecules as in combination therapy or polytherapy.

We report on a smart application of carbon nanotubes for kinetic stabilization of lipid particles that contain self-assembled nanostructures in their cores. The preparation of lipid particles requires rather low concentrations of carbon nanotubes permitting their use in biomedical applications such as drug delivery.

カーボンナノチューブにより安定化内部自己組織化脂質粒子の簡便な調製

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled ...

Facile Preparation of 4-Substituted Quinazoline Derivatives

Reported in this paper is a very simple method for direct preparation of 4-substituted quinazoline derivatives from a reaction between substituted 2-aminobenzophenones and thiourea in the presence of dimethyl sulfoxide (DMSO). This is a unique complementary reaction system in which thiourea undergoes thermal decomposition to form carbodiimide and hydrogen sulfide, where the former reacts with 2-aminobenzophenone to form 4-phenylquinazolin-2(1H)-imine intermediate, whilst hydrogen sulfide reacts with DMSO to give methanethiol or other sulfur-containing molecule which then functions as a complementary reducing agent to reduce 4-phenylquinazolin-2(1H)-imine intermediate into 4-phenyl-1,2-dihydroquinazolin-2-amine. Subsequently, the elimination of ammonia from 4-phenyl-1,2-dihydroquinazolin-2-amine affords substituted quinazoline derivative. This reaction usually gives quinazoline derivative as a single product arising from 2-aminobenzophenone as monitored by GC/MS analysis, along with small amount of sulfur-containing molecules such as dimethyl disulfide, dimethyl trisulfide, etc. The reaction usually completes in 4-6 hr at 160 &#186;C in small scale but may last over 24 hr when carried out in large scale. The reaction product can be easily purified by means of washing off DMSO with water followed by column chromatography or thin layer chromatography.

A protocol for facile preparation of 4-substituted quinazoline derivatives from 2-aminobenzophenones, thiourea and dimethyl sulfoxide is presented.

4-置換キナゾリン誘導体の簡便な準備

Reported in this paper is a very simple method for direct preparation of 4-substituted quinazoline derivatives from a reaction between substituted ...

Visualization of Ambient Mass Spectrometry with the Use of Schlieren Photography

This manuscript outlines how to visualize mass spectrometry ambient ionization sources using schlieren photography. In order to properly optimize the mass spectrometer, it is necessary to characterize and understand the physical principles of the source. Most commercial ambient ionization sources utilize jets of nitrogen, helium, or atmospheric air to facilitate the ionization of the analyte. As a consequence, schlieren photography can be used to visualize the gas streams by exploiting the differences in refractive index between the streams and ambient air for visualization in real time. The basic setup requires a camera, mirror, flashlight, and razor blade. When properly configured, a real time image of the source is observed by watching its reflection. This allows for insight into the mechanism of action in the source, and pathways to its optimization can be elucidated. Light is shed on an otherwise invisible situation.

This paper presents a protocol for the visualization of gaseous streams of an ambient ionization source using schlieren photography and mass spectrometry.

シュリーレン写真の使用とアンビエント質量分析の可視化

This manuscript outlines how to visualize mass spectrometry ambient ionization sources using schlieren photography. In order to properly optimize the mass ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

Photoredox触媒を用いた可視光媒介分散重合によるワームのようなミセルの簡便な合成

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Facile Preparation of (2Z,4E)-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high atomic and step economy. However, this functionality-directed cross-coupling reaction has not been developed, as there are still limited directing groups in practical use. In particular, a stoichiometric amount of oxidant is usually required, producing a large amount of waste. Due to our interest in novel 1,3-butadiene synthesis, we describe the ruthenium-catalyzed olefination of electron-deficient alkenes using allyl acetate and without external oxidant. The reaction of 2-phenyl acrylamide and allyl acetate was chosen as a model reaction, and the desired diene product was obtained in 80% isolated yield with good stereoselectivity (Z,E/Z,Z = 88:12) under optimal conditions: [Ru(p-cymene) Cl2]2 (3 mol %) and AgSbF6 (20 mol %) in DCE at 110 &#186;C for 16 h. With the optimized catalytic conditions in hand, representative &#945;- and/or &#946;-substituted acrylamides were investigated, and all reacted smoothly, regardless of aliphatic or aromatic groups. Also, differently N-substituted acrylamides have proven to be good substrates. Moreover, we examined the reactivity of different allyl derivatives, suggesting that the chelation of acetate oxygen to the metal is crucial for the catalytic process. Deuterium-labeled experiments were also conducted to investigate the reaction mechanism. Only Z-selective H/D exchanges on acrylamide were observed, indicating a reversible cyclometalation event. In addition, a kinetic isotope effect (KIE) of 3.2 was observed in the intermolecular isotopic study, suggesting that the olefinic C-H metalation step is probably involved in the rate-determining step.

Facile Preparation of 2Z,4E-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

The ruthenium-catalyzed olefination of electron-deficient alkenes with allyl acetate is described here. By using aminocarbonyl as a directing group, this external oxidant-free protocol has high efficiency and good stereo- and regioselectivity, opening a novel synthetic route to (Z,E)-butadiene skeletons.

（2<em&gt; Z</em&gt;、4<em&gt; E</em&gt;） - 電子不足アルケンと酢酸アリルとの合成によるジエナミド

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high ...