作者要感谢法国ANR（补助ANR-10-BLAN-0810 NEQSON）和CEA /丹麦/马尔库尔。

1，测量铀声致发光的在恒温的圆柱形sonoreactor被安装在高频换能器提供203或607千赫的超声波的顶部。超声波照射与低频超声的20千赫与一个1-cm 2的钛喇叭再现地放置在反应器的顶部进行。的发射光谱是使用耦合到光谱仪中记录范围230-800纳米的液氮冷却的CCD相机。氢在出口气体使用四极质谱仪（MS）的光谱研究同时进行测量。 <ol><li>通过紧密地附着在玻璃部件上的高频换能器和特氟隆盖保持在20千赫喇叭到玻璃部件准备sonoreactor。把sonoreactor上平移台，并与两个反射镜在反应器的中心调节其以图像的位置上发射光谱仪的入射狭缝。 </l我&gt; <li>通过将加权的UO 3的样品，通过CETAMA / CEA法国提供，在浓的HClO 4在加热条件下的最小体积制备在高氯酸铀酰溶液。然后调节溶液稀释高氯酸的体积。以制备铀酰溶液中的H 3 PO 4溶解UO在浓的HClO 4 3样品，蒸发得到的溶液至湿盐和溶解后者在0.5 MH 3 PO 4所需的音量。 </li><li>把解决方案，深入研究了sonoreactor。紧紧更换20 kHz的号角。添加热电偶和入口气体管上sonoreactor和出口气体管连接到质谱仪的入口。 </li><li>放在低温恒温器在〜0-1°C。让氩气泡在溶液以100毫升/分钟，至少30分钟的流速，开始以下的Ar和H 2的MS信号。 </li><li>当MS的信号是恒定的，接通超声波发生器（无论是高频的，在60〜80瓦特，或在20千赫1，在35瓦），并等待大约20分钟，直至约10℃的稳态温度达到sonoreactor内。在H 2 MS信号应该增加，说明空化和水超声降解。 </li><li>关闭该不透光的盒周围的sonoreactor并开始测量声致发光光谱，每个过程300秒，以确保良好的信号强度。对每个波长区间使3光谱来增加信噪比，并把第二阶光过滤器，如果必要。 </li><li>测量SL谱后，关掉超声波发生器和保持测量的MS信号，直到一个很好的基线为止。在同一时间，测量的发射光谱在没有美国的，这将允许以校正寄生虫光SL光谱。 </li></ol> 2，在水溶液中（四）超声化学还原的Pt <ol><li>制备由H 2 &lt;开始5克/升的Pt（IV）的溶液/ sub&gt;的PTCL 6·6H 2 O盐。备注：铂盐是光照和水分敏感。保留剩余的盐惰性气氛下，如果可能的话，进行加权过程中的非活性气体气氛手套箱。 </li><li>在通风橱中，设置了配有双套（ 图6），50毫升密闭的玻璃反应器。 <img alt="图6" fo:content-width="5in" src="/files/ftp_upload/51237/51237fig6highres.jpg" width="500" /> 图6：20千赫的超声波与750 实验装置为铂（IV）的声化学还原在20千赫1超声波发生器的最大电功率，2压电陶瓷换能器，3钛合金变幅杆，4恒温反应器中，W 5。 ，进气口，6，样品出口，7。热电偶，8。聚四氟乙烯环。 </li><li>装备的反应器中使用Pt-100热夫妇，隔垫，将PTFE气体入口和也为100毫升/分钟的范围内进行校准流量计的气体出口。出气口连接到水器（分子筛），最后到气体质谱仪注意：一定要抽空气体的通风橱内，因为二氧化碳是一种非常有害的化合物。在实验室中的CO气体检测仪是强制性的。 </li><li>在反应器的顶部，固定为1平方厘米钛探头由一个20千赫发生器提供一个压电换能器。确保该超声焊极尖是在从反应器的底部周围2厘米。 </li><li>在实验之前，启动制冷机，并设置温度为-18°C。在此期间，引入50ml去离子水的反应器内，使氩气/二氧化碳（10％）气体鼓泡深的溶液内以流速约100毫升/分钟。确保不存在重大的泄漏检查气体出口流速。肯定的是，超声焊极尖是1到2厘米的表面下液体和启动气体产物的监测。 </li><li>后10〜15分钟，固定略低于液体表面上的气体入口和一次冷却器到达设定温度时，启动超声波照射为17瓦/毫升的声功率。 </li><li>经过超声波照射15〜20分钟，检查温度达到40°C左右的稳定状态如果不是，请更改冷却器设置，以满足这一要求。 </li><li>取H 2 PTCL 6溶液用装有不锈钢针头的注射器的帮助的精确量。通过隔膜仔细介绍针和超声探头尖端下方的气蚀区中注入该溶液。轻轻抽液和缩小，最后取1毫升样品洗出的注射器。重复采样步骤，按15〜30分钟固定的时间间隔。 </li><li>测量稀释的一后的Pt离子的溶液用ICP-OES分析的总浓度的演变liquots在0.3M的硝酸 。在此期间，确定的Pt（IV）由260 nm的波段中的UV / Vis光谱学以下系统内离子的量。 </li><li>一旦没有了铂金离子可以在溶液中被检测到，关掉超声波照射，关闭气体鼓泡和冷水机组。取铂纳米颗粒悬浮液从反应器中。 </li><li>在此之前TEM分析，试图离心悬浮在高转速（20,414 XG）至少20分钟。小心地取出上清液，并存储存于室温下在真空下干燥后，或在少量的水离开它。 </li><li>一些样品可能是非常难以集中，并且可以不再需要离心时间。如果不成功，则使用该过程只对铂纳米粒子从超声波辐照过程中释放在溶液中的更大的氧化钛粒子分离，然后保持上清液这个时候。 </li><li>驱散一滴上清液或几毫克的无水乙醇或异丙醇干燥产品。存款悬挂一滴在碳包覆铜网格，进行溶剂的总蒸发后的高分辨透射电子显微镜分析。 </li></ol> 3，超声化学钚胶体的合成在马尔库尔，该ATALANTE设施配备几个热点实验室和屏蔽细胞系专用于研究和开发核燃料循环。其中一个手套箱致力于锕系元素的声化学反应的研究。 <ol><li>在50毫升的纯净水在位于手套箱内的声化学反应器中悬浮200毫克二氧化钚的（S BET = 13.3米2 /克）。 </li><li>装备的反应器与紧特氟隆环和20千赫的超声波探头。每次实验之前，螺钉一个新的提示，以确保气穴的最大效果和避免钛颗粒在从尖端侵蚀所得溶液的积累。 </li&gt; <li>设置位于手套箱足够低的超声后的温度管理增加溶液将被接通的外部的低温恒温器（胡伯CC1）的温度。注意，该冷却系统配备有一个热交换器，以避免阻挡外界放射性污染。插入紧热电偶进入细胞内，以控制溶液的温度。 </li><li>允许超声（100毫升/分钟）前20分钟用纯氩气冒泡的解决方案。需要注意的是，上述Ar鼓泡将在整个实验中超声处理可以应用于确保声空化的最大的效果。 </li><li>为了获得所需要的声功率P AC输送到溶液（17瓦/厘米2），该超声波发生器设置为适当的振幅（〜30％）。请注意，声功率是使用热探针法22以前测量。使用适当的条件下，过氧化氢在溶液中积累（导致从诱导的超声处理的水分子）的均裂分解羟基自由基的组合被预先在纯水中的测量来校准该系统，并允许在实验的再现性。 </li><li>接通超声波发生器和超声处理的二氧化钚的解决方案。调节低温恒温器设定，以获得在30℃的溶液温度下进行。 </li><li>一旦胶体（后5-12小时照射）形成的，在10分钟（22,000×g离心）关断的超声波发生器，将溶液转移到离心管中，离心分离，以除去固相。 </li><li>紫外可见分光光度计此后可以用于胶体浦直接分析和表征。在超声处理中，H 2的动力学O 2积累在超声辐射下，溶液也可以通过比色法在410nm（ε= 780nm -1 M -1）稀释500μl的样品溶液后，测定用500μlTiOSO 4（2×10 -2 M在2M的硝酸 - 0.01 M [N 2 H 5] [NO 3]），接着通过离心分离。 </li></ol>

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对于成功的观测声致发光和超声化学的最关键的参数是：1）严格控制的饱和气体和超声处理过程中的整体温度，2）仔细选择超声波频率，3）用超声处理溶液的最佳组合物，以防止淬火。 声化学反应的动力学以及声致发光的强度是提交给超声溶液的温度非常敏感：在对比最“通常”的化学反应的动力学的声化学过程的速率下降到与大容量的温度1。在声致发光显示出?...

在许多工业和研究领域，如固体表面的清洗，液体脱气，材料科学，环境整治和医学中的应用功率超声，已收到在过去十年中1多的关注。超声波处理提高了转换，提高了产率，并启动在均相溶液，以及在异构系统的反应。人们普遍认为在液体中的超声波振动的物理和化学效应源于声空化或者，换句话说，对微泡中的液体照射功率超声2的内爆塌陷。空化泡的内爆猛烈产生的瞬态极端条件中的气泡的气相，这是负责化学活性物质与声致发光的形成。然而，争论仍然继续在这样的极端条件下的原产地。光谱产品分析在声致发光第有助于更好地理解泡沫崩溃时发生的过程。在水，用惰性气体饱和时，声致发光光谱从俄亥俄州组成（A 2Σ+-X 2ΠI），俄亥俄州（C 2 S + A 2 S +）频段和广阔的统一体，从紫外到近红外部分的发射光谱3。俄亥俄州的光谱分析（A 2Σ+-X 2ΠI）发射带非平衡等离子体水4，5超声降解过程中发现的形成。在低超声频率，弱激发等离子体与布劳振动分布形成。与此相反，在高频率的超声波，里面塌陷等离子气泡展品特雷纳行为典型的强振动激发。该电子振动温度（T V，T五）增加与超声波的频率表明在更激烈的intrabubble条件高高频超声。 原则上，每个空化气泡可以被视为等离子体化学微反应器提供高能量的过程在本体溶液中的几乎室温。光子和气泡内产生的“热”的颗粒使激发非挥发性物质在溶液中从而增加了它们的化学反应性。例如，在酸性溶液中铀离子的超亮声致发光的机理受铀的浓度：通过光子碰撞的“热”的颗粒的吸收/再发射在稀释溶液，并激励有助于在更高的双氧铀的浓度6。由空化气泡产生的化学物种可以用于金属纳米颗粒的合成中，没有任何模板或封端剂。在纯水中通入氩气，在声化学还原的Pt（IV）的发生通过从声化学水分子分裂，得到单分散nanopartic发出氢莱金属铂7。声化学还原反应加速的歧管中的甲酸或Ar / CO气体混合物的存在下进行。 许多以前的研究表明超声的优势来激活分散固体的表面由于除了化学活化8,9力学效应。小固体颗粒小得多的尺寸比空化气泡不会扰乱崩溃的对称性。然而，当气穴的事件发生在靠近大聚集体或附近的延伸表面的气泡内爆不对称，形成超音速微喷导致簇解聚和于固体表面的侵蚀。超声处理使二氧化钚在纯水中通入氩气形成的原因钚（IV）的纳米胶体稳定，由于物理和化学作用10。

<table border="0" cellpadding="0" cellspacing="0" width="573">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">20 kHz Ultrasound Generator</td>
			<td style="width:71px;">Sonics Vibracell</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:216px;">Multifrequency Generator AG 1006</td>
			<td style="width:71px;">T&#38;C Power&#160; Conversion</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Cryostat RE210&#160;</td>
			<td style="width:71px;">Lauda</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Spectrometer SP 2356i</td>
			<td style="width:71px;">Roper Scientific</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">CCD camera SPEC10-100BR cooled with liquid nitrogen</td>
			<td style="width:71px;">Roper Scientific</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Quadrupole mass-spectrometer PROLAB 300</td>
			<td style="width:71px;">Thermoscientific</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Centrifuge Sigma 1-14</td>
			<td style="width:71px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">H2PtCl6 6H2O</td>
			<td style="width:71px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Ar; Ar/CO gases</td>
			<td style="width:71px;">Air Liquid</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Uranium and Plutonium compounds</td>
			<td style="width:71px;"></td>
			<td style="width:119px;"></td>
			<td>Prepared in the laboratories of Marcoule Research Center</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Perchloric acid</td>
			<td style="width:71px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Phosphoric acid</td>
			<td style="width:71px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Formic acid</td>
			<td style="width:71px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

activating molecules, ions, and solid particles with acoustic cavitation

化学和超声波的物理效应的产生不是由分子的直接相互作用与声波，而是从声空化：成核，生长，而在提交给功率超声微泡液体的内爆崩溃。气泡的剧烈的内爆导致化学反应的物质的形成，以及光，名为声致发光的发光。在这个手稿中，我们描述的技术允许极端intrabubble条件及声空化的解决方案化学反应的研究。水通入惰性气体声致发光光谱的分析提供了证据，非平衡等离子体形成。光子和空化气泡产生的“热”的颗粒使激发非挥发性物质在溶液中增加它们的化学反应性。例如，在酸性溶液中铀酰离子的超亮声致发光的机理与铀的浓度变化：sonophotoluminescence占主导地位的稀释溶液，并碰撞激发有利于在更高浓度的铀。次级声化学制品可能产生的气泡内部中形成的化学活性物质，但随后扩散到液相中，并与溶液中的前体反应形成的各种产品。例如，在纯水中的声化学还原的Pt（IV）的提供了一种创新的合成路线为金属铂的单分散纳米颗粒，没有任何模板或封端剂。许多研究显示超声的优势来激活分散固体。在一般情况下，超声波的机械效应强烈地在异构系统有助于除了化学效应。特别是， 二氧化钚粉末在纯水中的产量钚的稳定胶体，由于这两种效应的超声降解。

铀酰离子声致发光是极其微弱的高氯酸溶液：虽然典型的光吸收UO 2 2 +离子被观察到小于500 nm，发射距离兴奋线（UO 2 2 +）*（中心在512 nm和537 nm）的几乎不可见（ 图1）。 UO 2 2 +的SL被淬灭。此淬灭可以归因于由一个配位水分子减少11-13激发铀离子的： （UO 2 2 +）*</s...

Watch this Scientific Journal Video about Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation at JoVE.com

Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation

在提交给功率超声液体声空化产生的气泡崩溃瞬间内极端条件下，这是不寻常的化学反应和光发射，被称为声致发光的起源。在惰性气体的存在下，非平衡等离子体形成。通过塌缩的气泡所产生的“热点”粒子和光子能在溶液中激发物种。

活化分子，离子和固体颗粒与声空化

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

activating-molecules-ions-and-solid-particles-with-acoustic-cavitation

Research

JoVE Journal

Chemistry

15.0K 次观看.  UMR 5257 CEA-CNRS-UM2-ENSCM. 在提交给功率超声液体声空化产生的气泡崩溃瞬间内极端条件下，这是不寻常的化学反应和光发射，被称为声致发光的起源。在惰性气体的存在下，非平衡等离子体形成。通过塌缩的气泡所产生的“热点”粒子和光子能在溶液中激发物种。 

视频: Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation

Origami Inspired Self-assembly of Patterned and Reconfigurable Particles

There are numerous techniques such as photolithography, electron-beam lithography and soft-lithography that can be used to precisely pattern two dimensional (2D) structures. These technologies are mature, offer high precision and many of them can be implemented in a high-throughput manner. We leverage the advantages of planar lithography and combine them with self-folding methods1-20 wherein physical forces derived from surface tension or residual stress, are used to curve or fold planar structures into three dimensional (3D) structures. In doing so, we make it possible to mass produce precisely patterned static and reconfigurable particles that are challenging to synthesize.
In this paper, we detail visualized experimental protocols to create patterned particles, notably, (a) permanently bonded, hollow, polyhedra that self-assemble and self-seal due to the minimization of surface energy of liquefied hinges21-23 and (b) grippers that self-fold due to residual stress powered hinges24,25. The specific protocol described can be used to create particles with overall sizes ranging from the micrometer to the centimeter length scales. Further, arbitrary patterns can be defined on the surfaces of the particles of importance in colloidal science, electronics, optics and medicine. More generally, the concept of self-assembling mechanically rigid particles with self-sealing hinges is applicable, with some process modifications, to the creation of particles at even smaller, 100 nm length scales22, 26 and with a range of materials including metals21, semiconductors9 and polymers27. With respect to residual stress powered actuation of reconfigurable grasping devices, our specific protocol utilizes chromium hinges of relevance to devices with sizes ranging from 100 &mu;m to 2.5 mm. However, more generally, the concept of such tether-free residual stress powered actuation can be used with alternate high-stress materials such as heteroepitaxially deposited semiconductor films5,7 to possibly create even smaller nanoscale grasping devices.

We describe experimental details of the synthesis of patterned and reconfigurable particles from two dimensional (2D) precursors. This methodology can be used to create particles in a variety of shapes including polyhedra and grasping devices at length scales ranging from the micro to centimeter scale.

折纸灵感的图案和可重构颗粒自组装

There are numerous techniques such as photolithography, electron-beam lithography and soft-lithography that can be used to precisely pattern two ...

科研

化学

Dynamic Electrochemical Measurement of Chloride Ions

This protocol describes the dynamic measurement of chloride ions using the transition time of a silver silver chloride (Ag/AgCl) electrode. Silver silver chloride electrode is used extensively for potentiometric measurement of chloride ions concentration in electrolyte. In this measurement, long-term and continuous monitoring is limited due to the inherent drift and the requirement of a stable reference electrode. We utilized the chronopotentiometric approach to minimize drift and avoid the use of a conventional reference electrode. A galvanostatic pulse is applied to an Ag/AgCl electrode which initiates a faradic reaction depleting the Cl&#713; ions near the electrode surface. The transition time, which is the time to completely deplete the ions near the electrode surface, is a function of the ion concentration, given by the Nernst equation. The square root of the transition time is in linear relation to the chloride ion concentration. Drift of the response over two weeks is negligible (59 &#181;M/day) when measuring 1 mM [Cl&#713;]using a current pulse of 10 Am-2. This is a dynamic measurement where the moment of transition time determines the response and thus is independent of the absolute potential. Any metal wire can be used as a pseudo-reference electrode, making this approach feasible for long-term measurement inside concrete structures.

Dynamic measurement of chloride ions is presented. Transition time of an Ag/AgCl electrode, during a chronopotentiometric technique, can give the concentration of chloride ions in electrolyte. This method does not require a stable conventional reference electrode.

氯离子的动态电化学测试

This protocol describes the dynamic measurement of chloride ions using the transition time of a silver silver chloride (Ag/AgCl) electrode. Silver silver ...

X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder diffraction (XRPD) is presented in detail via two case studies.
The first material under investigation was sodium copper formate hydroxide oxide hydrate, Cu4Na4O(HCOO)8(OH)2&#8729;4H2O (sample 1) which forms on soda glass/copper alloy composite historic objects (e.g., enamels) in museum collections, exposed to formaldehyde and formic acid emitted from wooden storage cabinets, adhesives, etc. This degradation phenomenon has recently been characterized as &#34;glass induced metal corrosion&#34;.
For the second case study, thecotrichite, Ca3(CH3COO)3Cl(NO3)2&#8729;6H2O (sample 2), was chosen, which is an efflorescent salt forming needlelike crystallites on tiles and limestone objects which are stored in wooden cabinets and display cases. In this case, the wood acts as source for acetic acid which reacts with soluble chloride and nitrate salts from the artifact or its environment.
The knowledge of the geometrical structure helps conservation science to better understand production and decay reactions and to allow for full quantitative analysis in the frequent case of mixtures.

Modern high resolution X-ray powder diffraction (XRPD) in the laboratory is used as an efficient tool to determine crystal structures of long-known corrosion products on historic objects.

X射线粉末衍射在保护科学：迈向文物艺术品腐蚀产物的常规晶体结构测定

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

Measurement of Particle Size Distribution in Turbid Solutions by Dynamic Light Scattering Microscopy

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a technique used to measure the size distribution of polymer solutions or colloidal particles. Although this technique is widely used for the assessment of polymer solutions, it is difficult to measure the particle size in concentrated solutions due to the multiple scattering effect or strong light absorption. Therefore, the concentrated solutions should be diluted before measurement. Implementation of the confocal optical component in a dynamic light scattering microscope1 helps to overcome this barrier. Using such a microscopic system, both transparent and turbid systems can be analyzed under the same experimental setup without a dilution. As a representative example, a size distribution measurement of a temperature-responsive polymer solution was performed. The sizes of the polymer chains in an aqueous solution were several tens of nanometers at a temperature below the lower critical solution temperature (LCST). In contrast, the sizes increased to more than 1.0 &#181;m when above the LCST. This result is consistent with the observation that the solution turned turbid above the LCST.

A protocol for the direct measurement of particle size distribution in concentrated solutions using dynamic light scattering microscopy is presented.

通过动态光散射显微镜混浊解决方案粒度分布的测定

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a ...

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

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 of aqueous aluminum salts is known to produce a wide array of products with a wide range of size distributions, a variety of state-of-the-art instruments (i.e., 27Al/1H NMR, FTIR, ICP-OES, TEM-EDX, XPS, XRD, and BET) were used to characterize the synthesis products and identification of byproducts. The product, which was comprised of nanoparticles (10-30 nm), was isolated using gel permeation chromatography (GPC) column technique. Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffraction (PXRD) identified the purified material as the gibbsite polymorph of aluminum hydroxide. The addition of inorganic salts (e.g., NaCl) induced electrostatic destabilization of the suspension, thereby agglomerating the nanoparticles to yield Al(OH)3 precipitate with large particle sizes. By utilizing the novel synthetic method described here, Al(OH)3 was partially loaded inside the highly ordered mesoporous framework of MCM-41, with average pore dimensions of 2.7 nm, producing an aluminosilicate material with both octahedral and tetrahedral Al (Oh/Td = 1.4). The total Al content, measured using energy-dispersive X-ray spectrometry (EDX), was 11% w/w with a Si/Al molar ratio of 2.9. A comparison of bulk EDX with surface X-ray photoelectron spectroscopy (XPS) elemental analysis provided insight into the distribution of Al within the aluminosilicate material. Furthermore, a higher ratio of Si/Al was observed on the external surface (3.6) as compared to the bulk (2.9). Approximations of O/Al ratios suggest a higher concentration of Al(O)3 and Al(O)4 groups near the core and external surface, respectively. The newly developed synthesis of Al-MCM-41 yields a relatively high Al content while maintaining the integrity of the ordered silica framework and can be used for applications where hydrated or anhydrous Al2O3 nanoparticles are advantageous.

An ultrafine aluminum hydroxide nanoparticle suspension was prepared via the controlled titration of [Al(H2O)]3+ with L-arginine to pH 4.6 with and without cage-effect confinement within mesoporous channels of MCM-41.

在环境环境中制备具有或不具有介孔MCM-41的超细氢氧化铝颗粒

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 ...

Preparation of Stable Bicyclic Aziridinium Ions and Their Ring-Opening for the Synthesis of Azaheterocycles

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the aziridine ring. The utility of bicyclic aziridinium ions, specifically 1-azoniabicyclo[3.1.0]hexane and 1-azoniabicyclo[4.1.0]heptane tosylate highlighted in the aziridine ring openings by the nucleophile with the release of the ring strain to yield the corresponding ring-expanded azaheterocycles such as pyrrolidine, piperidine and azepane with diverse substituents on the ring in regio- and stereospecific manner. Herein, we report a simple and convenient method for the preparation of the stable 1-azabicyclo[4.1.0]heptane tosylate followed by selective ring opening via a nucleophilic attack either at the bridge or at the bridgehead carbon to yield piperidine and azepane rings, respectively. This synthetic strategy allowed us to prepare biologically active natural products containing piperidine and azepane motif including sedamine, allosedamine, fagomine and balanol in highly efficient manner.

Bicyclic aziridinium ions such as 1-azoniabicyclo[4.1.0]heptane tosylate were generated from 2-[4-tolenesulfonyloxybutyl]aziridine, which was utilized for the preparation of substituted piperidines and azepanes via regio- and stereospecific ring-expansion with various nucleophiles. This highly efficient protocol allowed us to prepare diverse azaheterocycles including natural products such as fagomine, febrifugine analogue and balanol.

稳定笼 Aziridinium 离子的制备及其开环 Azaheterocycles 的合成

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of solid-phase synthesis, regenerating Michael (REM) linker strategies, and 1,3-dipolar cycloaddition, a library of structurally similar heterocycles, both with and without a spirocyclic center, can be constructed. The main advantages of the solid-support synthesis are as follows: first, each reaction step can be driven to completion using a large excess of reagents resulting in high yields; next, the use of commercially available starting materials and reagents keep the costs low; finally, the reaction steps are easy to purify via simple filtration. The REM linker strategy is attractive because of its recyclability and traceless nature. Once a reaction scheme is completed, the linker can be reused multiple times. In a typical solid-phase synthesis, the product contains either a part of or the whole linker, which can prove undesirable. The REM linker is &#34;traceless&#34; and the point of attachment between the product and the polymer is indistinguishable. The high diastereoselectivity of the intramolecular 1,3-dipolar cycloaddition is well documented. Limited by the insolubility of the solid support, the reaction progression can only be monitored by a change in the functional groups (if any) via infrared (IR) spectroscopy. Thus, the structural identification of intermediates cannot be characterized by conventional nuclear magnetic resonance (NMR) spectroscopy. Other limitations to this method stem from the compatibilities of the polymer/linker to the desired chemical reaction scheme. Herein we report a protocol that allows for the convenient production of spirocyclic heterocycles that, with simple modifications, can be automated with high-throughput techniques.

Here we present a protocol to demonstrate an efficient method for the synthesis of spirocyclic heterocycles. The five-step process utilizes solid-phase synthesis and regenerating Michael linker strategies. Generally difficult to synthesize, we present a customizable method for the synthesis of spirocyclic molecules otherwise inaccessible to other modern approaches.

[4.4] 刺环氧基的固相合成

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of ...

Stable DNA Motifs, 1D and 2D Nanostructures Constructed from Small Circular DNA Molecules

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D DNA nanostructures. Over decades, the rapid development of DNA nanotechnology is attributed to the use of linear DNAs as the source materials. For example, the DAO (double crossover, antiparallel, odd half-turns) tile is well-known as a building block for construction of 2D DNA lattices; the core structure of DAO is made from two linear single-stranded (ss) oligonucleotides, like two ropes making a right hand granny&#160;knot. Herein, a new type of DNA tiles called cDAO (coupled DAO) are built using a small circular ss-DNA of c64nt or c84nt (circular 64 or 84 nucleotides) as the scaffold strand and several linear ss-DNAs as the staple strands. Perfect 1D and 2D nanostructures are assembled from cDAO tiles: infinite nanowires, nanospirals, nanotubes, nanoribbons; and finite nano-rectangles. Detailed protocols are described: 1) preparation by T4 ligase and purification by denaturing PAGE (polyacrylamide gel electrophoresis) of small circular oligonucleotides, 2) annealing of stable circular tiles, followed by native PAGE analysis, 3) assembling of infinite 1D nanowires, nanorings, nanospirals, infinite 2D lattices of nanotubes and nanoribbons, and finite 2D nano-rectangles, followed by AFM (Atomic Force Microscopy) imaging. The method is simple, robust, and affordable for most labs.

This article presents a detailed protocol for T4 ligation and denaturing PAGE purification of small circular DNA molecules, annealing and native PAGE analysis of circular tiles, assembling and AFM imaging of 1D and 2D DNA nanostructures, as well as agarose gel electrophoresis and centrifugation purification of finite DNA nanostructures.

由小圆形 DNA 分子构建的稳定 DNA 分子、一维和二维纳米结构

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D ...

Accumulation and Analysis of Cuprous Ions in a Copper Sulfate Plating Solution

Knowledge of the behavior of cuprous ions (monovalent copper ion: Cu(I)) in a copper sulfate plating bath is important for improving the plating process. We successfully developed a method to quantitatively and easily measure Cu(I) in a plating solution and used it for evaluation of the solution. In this paper, a quantitative absorption spectrum measurement and a time-resolved injection measurement of Cu(I) concentrations by a color reaction are described. This procedure is effective as a method to reproduce and elucidate the phenomenon occurring in the plating bath in the laboratory. First, the formation and accumulation process of Cu(I) in solution by electrolysis of a plating solution is shown. The amount of Cu(I) in the solution is increased by electrolysis at higher current values &#8203;&#8203;than the usual plating process. For the determination of Cu(I), BCS (bathocuproinedisulfonic acid, disodium salt), a reagent that selectively reacts with Cu(I), is used. The concentration of Cu(I) can be calculated from the absorbance of the Cu(I)-BCS complex. Next, the time measurement of the color reaction is described. The color reaction curve of Cu(I) and BCS measured by the injection method can be decomposed into an instantaneous component and a delay component. By analysis of these components, the holding structure of Cu(I) can be clarified, and this information is important when predicting the quality of the plating film to be produced. This method is used to facilitate the evaluation of the plating bath in the production line.

Here, accumulation of cuprous ions in a copper sulfate plating solution in a model experiment and an analysis based on quantitative measurements are described. This experiment reproduces the accumulation process of cuprous ions in the plating bath.

硫酸铜镀液中铜离子的积累与分析

Knowledge of the behavior of cuprous ions (monovalent copper ion: Cu(I)) in a copper sulfate plating bath is important for improving the plating process. ...