这项工作是由欧洲燃料电池和Hydruogen联合执行下的合作项目BOR4STORE（批准号:303428协定）和基础设施项目H2FC（赠款协​​议号FP7-284522）的支持。

1.仪器<ol><li>使用由通过高压气体配管连接的四个主要部件的基本超临界干燥（SCD）装置:气体供应，真空系统，传感器（温度和压力），和样品环境（其可在浴中浸没）。确保建设优质不锈钢阀门，管件和管道，额定压力为至少10兆帕80-300 K之间的温度范围内 注意:示意图示于图1。 </li><li>对于氮理学博士（NSCD）处理，确保气源的纯度研究装有0-10兆帕之间的出口压力控制压力调节器（&gt; 99.999％）的氮气。附加一个50升瓶（20兆帕）的装置，并在使用前冲洗系统用纯氮气多次。 </li><li>保证真空系统能够实现真空压力下降到&lt;0.1帕的并且被连接到该装置与一精细控制针阀。优选地，使用无油粗抽泵和一个分子拖动涡轮泵，串联放置。 </li><li>使用至少两个压力传感器对压力的精确测量期间理学治疗:真空测量和高压力传感器的低压压力传感器来实现0.1-10 7帕之间的总测的压力范 ​​围。 </li><li>使用至少两个温度传感器，用于必要的最小的精度来执行典型理学治疗:与样品和77-300 K的主要气体计量歧管用于精确测量内的传感器热接触的传感器（ 例如 ，K型热电偶） 。 </li><li>检查该样本保持器必须包含必要的样品用于治疗的量的适当的内部容积，并且由不锈钢制成。 注:加长的圆柱形设计有助于同浴热接触。 </li><li>确保封闭该样本容器的嵌合是appropr黄昏时分的高压和重复使用（ 例如 ，世伟洛克VCR）。通过管道的适当长度（汲取管），用于样品支架的完全浸没入熔池连接样本容器容积的阀从外部环境隔离。 </li></ol><img alt="图1" src="/files/ftp_upload/52817/52817fig1.jpg" /> 在环境温度和（B）（A）中，在浴中的试样浸入后: 图1.超临界氮气干燥（NSCD）一种用于在典型的实验室使用简化NSCD装置的示意图。气体供应在这项工作中所描述的方法是氮，但是这一般装置推广到其他理学流体与一个临界点躺着的温度和压力，如CO 2的实用范围内。组件被标记为与第一致Ë这里所描述的协议。 <a href="https://www.jove.com/files/ftp_upload/52817/52817fig1highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 2.准备工作<ol><li>负载0.2-0.5克样品（γ-Mg系（BH 4）2，粉末形式，以下湿式化学合成和标准的干燥方法）到样本保持在适当条件下，通常在惰性气氛如氩气手套箱，在环境温度下或更低。关闭样品保持器（嵌合F2）与过滤器垫圈，然后关闭阀（阀V4）。样品架传送到装置和连接（嵌合F1）。 </li><li>打开计量歧管通过V2真空和撤离。打开V3和疏散。由V1用氮气净化的装置和经由V2撤离。开放V4和撤离样品在RT达24小时，以达到系统（&lt;0.1帕）的最小压力。 </li><li>安装示例浴（见<strong&gt;的图2）的样品架周围。通过提高浴到位上剪叉式升降机，或类似的机制执行此。 </li><li>设定加热到所需未来液体温度（T L，见步骤3.1）的110 K，并继续撤离设备直至温度达到平衡。 </li></ol><img alt="图2" src="/files/ftp_upload/52817/52817fig2.jpg" /> 图2.低温炉样品浴一个示意图（左）和一个cryostatic热浴环境照片（右）相应于含有NSCD处理期间的样品架，允许测量和77-298 K之间的样品温度控制<a href="https://www.jove.com/files/ftp_upload/52817/52817fig2highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 3.超临界氮曝光<ol&gt; <li>对于γ-Mg系（BH 4）2，（示范的在这个协议中的主题）的NSCD处理选择的110 K的液体温度（T L）这对应于一个中等的液体溶剂密度（〜0.6克毫升-1） ;在必要时获得本协议的其他NSCD治疗过程中的应用调整（见下面的注释）。 </li><li>通过关闭V2封闭该系统至真空。油门开V1慢，使压力提高到相图的液相区。平衡系统在2兆帕和T L。 </li><li>浸泡试样在液体N 2 4小时。 </li><li>与斜坡≤2，K MIN -1设置加热器150开。允许的压力增加不高于该装置的最大额定压力（此{P MAX应≥10兆帕）;如果必要的话，仔细地发泄过剩的压力，通过V2真空。平衡系统以P max和150 K. </li><li>泡在SUP样本ercritical N 2 1小时。 </li></ol><img alt="图3" src="/files/ftp_upload/52817/52817fig3.jpg" /> 图3.氮相图氮，这里的流体密度（如图线性灰度）详细的相图使用REFPROP（状态的修正韦伯-笃-鲁宾公式）计算。41多种线密度不变的示紫色。固相边界和沸腾过渡线被显示为红色。蓝线表示的相图是有关使用N 2干燥或提取加工的区域的边界。 <a href="https://www.jove.com/files/ftp_upload/52817/52817fig3highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 注意:对于此协议的其他材料的应用，建立适当的治疗NSCD舍姆Ë通过选择所需的目标物种的有效溶解的条件。指的是N 2的相图，在图3中所示，为了实现高的流体密度在液相（ 例如，0.8-1克·毫升-1），选择80-90 K.一件T l对于中等的液体密度（ 例如，0.6-0.8克·毫升-1），选择90-115 K的试错法一个T L可能是必要的。 4.超临界氮素释放<ol><li>仔细节流V2，使压力尽可能慢减少破解系统至真空。反复破解系统根据需要实现12-24小时的大致时间跨度逐渐下降到高真空（&lt;0.1 ​​Pa）的高真空率。 </li><li>取下样品浴缸和全开V2完全撤离样品。平衡在室温和高真空（&lt;0.1帕）。 </li><li>脱气样品在RT和&lt;0.1帕为1-24小时，为desired。 </li></ol> 5.后处理<ol><li>关闭阀门V3和V4，和从（嵌合F1），该装置移动样品支架。 </li><li>样品架传送到惰性环境进行处理，如在氩气填充的手套箱中。在密封容器中在环境温度下或低于除去从样品保持器（嵌合F2），并存储该样本。 </li></ol>

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G., Baricco, M., Bordiga, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fast+carbon+dioxide+recycling+by+reaction+with+&#947;-Mg(BH4)2.">Fast carbon dioxide recycling by reaction with &#947;-Mg(BH4)2.</a> Phys. Chem. Chem. Phys. 16, 22482-22486 (2014).</li><li>Paskevicius, M., 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=In-Situ+X-ray+Diffraction+Study+of+&#947;-Mg(BH4)2+Decomposition.">In-Situ X-ray Diffraction Study of &#947;-Mg(BH4)2 Decomposition.</a> J. Phys. Chem. C. 116, 15321-15240 (2012).</li><li>Lemmon, E. W., Huber, M. L., McLinden, M. O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NIST+standard+reference+database+23:+reference+fluid+thermodynamic+and+transport+properties.">NIST standard reference database 23: reference fluid thermodynamic and transport properties.</a> Standard Reference Data Program. , (2008).</li><li>Moquin, P. H. L., Temelli, F. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetic+modeling+of+hydrolysis+of+canola+oil+in+supercritical+media.">Kinetic modeling of hydrolysis of canola oil in supercritical media.</a> J. Supercrit. Fluid. 45, 94-101 (2008).</li><li>Myers, M. N., Giddings, 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=Ultra-High-Pressure+Gas+Chromatography+in+Micro+Columns+to+2000+Atmospheres.">Ultra-High-Pressure Gas Chromatography in Micro Columns to 2000 Atmospheres.</a> Sep. Sci. 1 (6), 761-776 (1966).</li><li>McLeary, E. E., Jansen, J. C., Kapteijn, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Zeolite+based+films,+membranes+and+membrane+reactors:+Progress+and+prospects.">Zeolite based films, membranes and membrane reactors: Progress and prospects.</a> Microporous Mesoporous Mater. 90, 198-220 (2006).</li><li>Richter, B., Ravnsb&#230;k, D. B., Tumanov, N., Filinchuk, Y., Jensen, T. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Manganese+borohydride;+synthesis+and+characterization.">Manganese borohydride; synthesis and characterization.</a> Dalton Trans. , (2015).</li><li>Liang, S., Tilotta, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extraction+of+petroleum+hydrocarbons+from+soil+using+supercritical+argon.">Extraction of petroleum hydrocarbons from soil using supercritical argon.</a> Anal. Chem. 70 (3), 616-622 (1998).</li></ol>

作者什么都没有透露。

这可能是由于其相对较低的临界温度（126 K），N 2 -历来被忽视作为有效理学溶剂。在早先的报告，3,17,42,43它仅被暗示在等于或高于室温，在那里它显示只有少量的溶剂化功率加工温度的范围内，由于其低的流体密度在其相图的这个区域（除在极高的压力，43）。在实现的N 2的实际效用作为超临界溶剂的关键步骤是在维持处理温度在临界点附近，那里的密度（因此?...

超临界流体萃取（SFE）和干燥（SCD）方法被很好地建立在广泛的实际应用，特别是在食品工业和石油工业，也可在化学合成，分析和材料的加工。1-6使用干燥或提取介质在高于其临界点条件往往是更快，更清洁和更有效的比传统的（液体）的技术，并具有可通过操作条件稍作调整相对于高度可调的流体的溶剂化功率的额外优点3,7一种简单的方法理学包括三个基本步骤。第一步是露出其包含在其液体中的目标杂质化合物来适当选择理学流体的固体（或者液体）的原料（或接近液体超临界相），在那里它的高密度对应于高（也许选择性7）溶剂功率相对于所述靶物种。 Ť他第二步骤加热和压缩上述所选理学流体的临界点，系统中的封闭容器，以使流体和其溶解靶物种不通过相界这可能导致分离。最后一步是缓慢降低理学流体的真空压力在高于临界温度的温度下，使含有目标物种逃脱，再次没有遇到一个相界或沿途的任何有害的表面张力作用的流体溶液。 起始原料为左耗尽目标物种的，并且可以进行迭代处理，如果有必要的。在超临界流体萃取的情况下，目标溶质种类是所需产物，并从供进一步使用的解决方案。8,9-收集在其他情况下，将干燥的或纯化的起始材料是期望的产物，并将所提取的杂质被丢弃。这后一种情况下，这里所指作为理学方法，被发现是一种有效的策略，高表面积，微孔材料，如金属 - 有机骨架（MOFs），其中，在真空下传统的热处理方法在许多情况下，在清除孔不充分的预处理所有的不速之客，或导致孔隙坍塌。10二氧化碳理学博士（CSCD）处理现在是一个常规的后期合成的过程MOFs材料，11导致增加氮可接触的表面面积比高达1000％未经处理的材料12其他的改进，如在催化活性。13其他值得注意的超临界流体的应用是作为一种广泛可调谐介质进行化学反应，14-16超临界流体色谱（SCFC）6,17,18和合成气凝胶和先进复合材料。19- 22 对于干燥应用，理学博士流体是基于两个标准来选择:一）接近它的临界点到环境的条件（为方便起见，并降低能源成本或处理复杂性）和b）其溶剂化功率相对于所述靶物种。二氧化碳（CO 2）已被证明是在许多应用中方便理学流体，因为它是无毒的，不可燃的，并且价格便宜，并且可以进行调节，以表现出高的溶剂化功率朝向一些普通的有机靶物种在其近液体的状态（在&lt;10兆帕的压力和温度273-323 K）1-3,7-9其他常见的超临界溶剂（或共溶剂）包括水（跨越一个显着的其环境和超临界状态之间溶剂性能范围23），丙酮，乙烯，甲醇，乙醇，和乙烷，覆盖从极性（质子和非质子传递）到非极性的，并具有对环境条件相对临界点附近的频谱。 二氧化碳是迄今为止最常用理学流体。在建立CSCD方法中，反应性的原料不是抑制因子，因为二氧化碳是只有非常弱的温度接近它的临界点的反应。然而，由于其在水或CO 2存在强的反应，除了在加热下其（可能故意量身定做）不稳定某些类的材料，如所谓的复合氢化物（ 例如 ，铝氢化物和硼氢化物）在处理本独特的挑战24-26此外，还有在这样的材料如高密度的储氢化合物，27-30极大国际兴趣，因此，可以在纳米结构和/或多孔的品种31-33。对于这样的反应性的，不稳定的，纳米结构材料的有效的净化，理学的方法是有前途的策略。34所述理学流体必须使用具有适用于穿入窄空腔分子直径小并且还具有高的溶剂化功率朝向目标杂质，WHI勒剩余朝向起始材料本身不反应。这里，利用超临界氮气（N 2）作为用于这种提取和特别干燥应用提供有效的流体呈现。具体超临界氮气干燥（NSCD）方法是下面描述的γ相镁硼氢化其中目标种类包括二硼烷和正丁基的化合物（类似但不专门识别为正丁烷）的纯化。下面的协议可以很容易地修改一般扩展到其他超临界氮气干燥或提取过程。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Compressed Nitrogen Gas</td>
			<td>Messer Schweiz AG</td>
			<td></td>
			<td>50 L bottle, purity &#62; 99.999%, &#60;3 ppmv H2O</td>
		</tr>
		<tr>
			<td>Liquid Nitrogen</td>
			<td>Pan Gas AG</td>
			<td></td>
			<td>Bulk storage, on site</td>
		</tr>
		<tr>
			<td>Custom Supercritical Drying Apparatus</td>
			<td>Empa</td>
			<td></td>
			<td>Swagelok (compression fitting and VCR) components</td>
		</tr>
		<tr>
			<td>Custom Cryogenic Furnace Bath</td>
			<td>Empa</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Custom Labview Interface</td>
			<td>Empa</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

supercritical nitrogen processing for the purification of reactive porous materials

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. Herein, nitrogen is presented as a novel supercritical drying fluid for specialized applications such as in the processing of reactive porous materials, where carbon dioxide and other fluids are not appropriate due to their higher chemical reactivity. Nitrogen exhibits similar physical properties in the near-critical region of its phase diagram as compared to carbon dioxide: a widely tunable density up to ~1 g ml-1, modest critical pressure (3.4 MPa), and small molecular diameter of ~3.6 &#197;. The key to achieving a high solvation power of nitrogen is to apply a processing temperature in the range of 80-150 K, where the density of nitrogen is an order of magnitude higher than at similar pressures near ambient temperature. The detailed solvation properties of nitrogen, and especially its selectivity, across a wide range of common target species of extraction still require further investigation. Herein we describe a protocol for the supercritical nitrogen processing of porous magnesium borohydride.

碱金属和碱土金属硼氢化物是潜在的储氢材料，其在分解。27,29其他分解产物递送气态氢的含量大，如乙硼烷也有时被解吸的气体中检测到，但其来源没有先验明确;有可能它们是纯相的分解产品，但也可以是杂质的杂质反应或产物剩从化学合成。35镁硼氢化的多孔相（γ-Mg系（BH 4）2）表现出既具有高比表面积（&gt; 1,000米2 g -1）以上和氢。36及其脱?...

Watch this Scientific Journal Video about Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials at JoVE.com

Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

氮气是用于萃取或干燥过程的有效的超临界流体，由于其小的分子尺寸，高密度在近液体超临界状态，和化学惰性。我们提出了一个超临界氮气干燥协议用于净化处理的反应性的，多孔的材料。

超临界氮处理的活性多孔材料的净化

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. ...

supercritical-nitrogen-processing-for-purification-reactive-porous

Research

JoVE Journal

Chemistry

14.6K 次观看.  Empa, Swiss Federal Laboratories for Materials Science and Technology. 氮气是用于萃取或干燥过程的有效的超临界流体，由于其小的分子尺寸，高密度在近液体超临界状态，和化学惰性。我们提出了一个超临界氮气干燥协议用于净化处理的反应性的，多孔的材料。 

视频: Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

Folding and Characterization of a Bio-responsive Robot from DNA Origami

The DNA nanorobot is a hollow hexagonal nanometric device, designed to open in response to specific stimuli and present cargo sequestered inside. Both stimuli and cargo can be tailored according to specific needs. Here we describe the DNA nanorobot fabrication protocol, with the use of the DNA origami technique. The procedure initiates by mixing short single-strand DNA staples into a stock mixture which is then added to a long, circular, single-strand DNA scaffold in presence of a folding buffer. A standard thermo cycler is programmed to gradually lower the mixing reaction temperature to facilitate the staples-to-scaffold annealing, which is the guiding force behind the folding of the nanorobot. Once the 60 hr folding reaction is complete, excess staples are discarded using a centrifugal filter, followed by visualization via agarose-gel electrophoresis (AGE). Finally, successful fabrication of the nanorobot is verified by transmission electron microscopy (TEM), with the use of uranyl-formate as negative stain.

DNA origami is a powerful method for fabricating precise nanoscale objects by programming the self-assembly of DNA molecules. Here we describe a protocol for the folding of a bio-responsive robot from DNA origami, its purification and negative staining for transmission electron microscopic imaging (TEM).

折叠的DNA折纸一个生物反应机器人与表征

The DNA nanorobot is a hollow hexagonal nanometric device, designed to open in response to specific stimuli and present cargo sequestered inside. Both ...

科研

化学

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

对磷酸增强富集制备高度多孔配位聚合物涂层的孔聚合物石柱的

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

在线含硫化合物在复杂油气矩阵氮分析

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Insights into the Interactions of Amino Acids and Peptides with Inorganic Materials Using Single-Molecule Force Spectroscopy

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals leads to the formation of composite materials with unique properties. In addition, the undesirable process of biofouling is initiated by the adsorption of biomolecules, mainly proteins, on surfaces. This organic layer is an adhesion layer for bacteria and allows them to interact with the surface. Understanding the fundamental forces that govern the interactions at the organic-inorganic interface is therefore important for many areas of research and could lead to the design of new materials for optical, mechanical and biomedical applications. This paper demonstrates a single-molecule force spectroscopy technique that utilizes an AFM to measure the adhesion force between either peptides or amino acids and well-defined inorganic surfaces. This technique involves a protocol for attaching the biomolecule to the AFM tip through a covalent flexible linker and single-molecule force spectroscopy measurements by atomic force microscope. In addition, an analysis of these measurements is included.

Here we present a protocol to measure the force of interactions between a well-defined inorganic surface and either peptides or amino acids by single-molecule force spectroscopy measurements using an atomic force microscope (AFM). The information obtained from the measurement is important to better understand the peptide-inorganic material interphase.

洞察氨基酸和多肽与无机材料的使用相互作用的单分子力谱

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

形状-各向异性胶体镉硫纳米结构的 Facet-to-facet 连接

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three preparation methods are described: (a) the incorporation of metal salts into silica or alumina wet gels using an impregnation method; (b) the incorporation of metal salts into alumina wet gels using a co-precursor method; and (c) the addition of metal nanoparticles directly into a silica aerogel precursor mixture. The methods utilize a hydraulic hot press, which allows for rapid (&#60;6 h) supercritical extraction and results in aerogels of low density (0.10 g/mL) and high surface area (200-800 m2/g). While the work presented here focuses on the use of copper salts and copper nanoparticles, the approach can be implemented using other metal salts and nanoparticles. A protocol for testing the three-way catalytic ability of these aerogels for automotive pollution mitigation is also presented. This technique uses custom-built equipment, the Union Catalytic Testbed (UCAT), in which a simulated exhaust mixture is passed over an aerogel sample at a controlled temperature and flow rate. The system is capable of measuring the ability of the catalytic aerogels, under both oxidizing and reducing conditions, to convert CO, NO and unburned hydrocarbons (HCs) to less harmful species (CO2, H2O and N2). Example catalytic results are presented for the aerogels described.

Here we present protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms. Methods for preparing materials using copper salts and copper-containing nanoparticles are featured. Catalytic testing protocols demonstrate the effectiveness of these aerogels for three-way catalysis applications.

快速超临界萃取制备催化气凝胶的制备与试验研究

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Deposition of Porous Sorbents on Fabric Supports

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material that can be subsequently treated by dip coating. Dip coating with a sol preparation provides a supported porous layer on the fabric. In this case, the porous layer is a porphyrin functionalized sorbent system based on a powdered material that has been demonstrated previously for the capture and conversion of phosgene. A representative coating is applied to cotton fabric at a loading level of 10 mg/g. This coating has minimal impact on water vapor transport through the fabric (93% of the support fabric rate) while significantly reducing transport of 2-chloroethyl ethyl sulfide (CEES) through the material (7% of support fabric rate). The described approaches are suitable for use with other fabrics providing amine and hydroxyl groups for modification and can be used in combination with other sol preparations to produce varying functionality.

This report details a microwave-initiated approach for deposition of porphyrin functionalized porous organosilicate sorbents on a cotton fabric and demonstrates reduction in 2-chloroethyl ethyl sulfide (CEES) transport through the fabric resulting from this treatment.

织物支架上多孔吸附剂的沉积

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its well-balanced ferroelectricity, piezoelectricity, and dielectric constant. In addition, BT does not contain any toxic elements. Therefore, it is considered to be an eco-friendly material, which has attracted considerable interest as a replacement for lead zirconate titanate (PZT). However, bulk BT loses its ferroelectricity at approximately 130 &#176;C, thus, it cannot be used at high temperatures. Because of the growing demand for high-temperature ferroelectric materials, it is important to enhance the thermal stability of ferroelectricity in BT. In previous studies, strain originating from the lattice mismatch at hetero-interfaces has been used. However, the sample preparation in this approach requires complicated and expensive physical processes, which are undesirable for practical applications.
In this study, we propose a chemical synthesis of a porous material as an alternative means of introducing strain. We synthesized a porous BT thin film using a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles were used as an organic template. Through a series of studies, we clarified that the introduction of pores had a similar effect on distorting the BT crystal lattice, to that of a hetero-interface, leading to the enhancement and stabilization of ferroelectricity. Owing to its simplicity and cost effectiveness, this fabrication process has considerable advantages over conventional methods.

Here, we present a protocol for the synthesis of porous barium titanate (BaTiO3) thin film by a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles are used as an organic template.

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

Synthesis and Bioconjugation of Thiol-Reactive Reagents for the Creation of Site-Selectively Modified Immunoconjugates

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. Yet maleimide-based conjugates display limited stability in vivo because the succinimidyl thioether linkage can undergo a retro-Michael reaction. This, of course, can lead to the release of the radioactive payload or its exchange with thiol-bearing biomolecules in circulation. Both of these processes can produce elevated activity concentrations in healthy organs as well as decreased activity concentrations in target tissues, resulting in reduced imaging contrast and lower therapeutic ratios. In 2018, we reported the creation of a modular, stable, and easily accessible phenyloxadiazolyl methyl sulfone reagent &#8212; dubbed &#8216;PODS&#8217; &#8212; as a platform for thiol-based bioconjugations. We have clearly demonstrated that PODS-based site-selective bioconjugations reproducibly and robustly create homogenous, well-defined, highly immunoreactive, and highly stable radioimmunoconjugates. Furthermore, preclinical experiments in murine models of colorectal cancer have shown that these site-selectively labeled radioimmunoconjugates exhibit far superior in vivo performance compared to radiolabeled antibodies synthesized via maleimide-based conjugations. In this protocol, we will describe the four-step synthesis of PODS, the creation of a bifunctional PODS-bearing variant of the ubiquitous chelator DOTA (PODS-DOTA), and the conjugation of PODS-DOTA to the HER2-targeting antibody trastuzumab.

In this protocol, we will describe the synthesis of PODS, a phenyoxadiazolyl methyl sulfone-based reagent for the site-selective attachment of cargos to the thiols of biomolecules, particularly antibodies. In addition, we will describe the synthesis and characterization of a PODS-bearing bifunctional chelator and its conjugation to a model antibody.

硫醇反应试剂的合成与生物共轭作用--用于原位选择性修饰免疫共轭的生成

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. ...

Evaluation of Oxidative Stress in Biological Samples Using the Thiobarbituric Acid Reactive Substances Assay

Despite its limited analytical specificity and ruggedness, the thiobarbituric acid reactive substances (TBARS) assay has been widely used as a generic metric of lipid peroxidation in biological fluids. It is often considered a good indicator of the levels of oxidative stress within a biological sample, provided that the sample has been properly handled and stored. The assay involves the reaction of lipid peroxidation products, primarily malondialdehyde (MDA), with thiobarbituric acid (TBA), which leads to the formation of MDA-TBA2 adducts called TBARS. TBARS yields a red-pink color that can be measured spectrophotometrically at 532 nm. The TBARS assay is performed under acidic conditions (pH = 4) and at 95 &#176;C. Pure MDA is unstable, but these conditions allow the release of MDA from MDA bis(dimethyl acetal), which is used as the analytical standard in this method. The TBARS assay is a straightforward method that can be completed in about 2 h. Preparation of assay reagents are described in detail here. Budget-conscious researchers can use these reagents for multiple experiments at a low cost rather than buying an expensive TBARS assay kit that only permits construction of a single standard curve (and thus can only be used for one experiment). The applicability of this TBARS assay is shown in human serum, low density lipoproteins, and cell lysates. The assay is consistent and reproducible, and limits of detection of 1.1 &#956;M can be reached. Recommendations for the use and interpretation of the spectrophotometric TBARS assay are provided.

The goal of the thiobarbituric acid reactive substances assay is to assess oxidative stress in biological samples by measuring the production of lipid peroxidation products, primarily malondialdehyde, using visible wavelength spectrophotometry at 532 nm. The method described here can be applied to human serum, cell lysates, and low density lipoproteins.

使用硫代巴比妥酸反应物质测定法评估生物样品中的氧化应激

Despite its limited analytical specificity and ruggedness, the thiobarbituric acid reactive substances (TBARS) assay has been widely used as a generic ...