我们承认化学的弗吉尼亚军事学院（VMI）处获得支持的电化学实验和仪器（LSC和JTH）。学院院长的办公室VMI与支持朱庇特的出版物相关的生产费用。我们承认UNC EFRC：中心太阳能燃料，由能源，科学办公室，基础能源科学根据奖号码DE-SC0001011办公室，美国能源部资助支持复合和合成材料的表征的能源前沿研究中心（DPH ）。

1.合成1 根据- ：合成1（图4; 5,5&#39;- dvbpy是5,5&#39;-二乙烯基-2,2&#39;-联吡啶三联吡啶，2&#39;&#39;PhTpy是4&#39;-苯基-2,2&#39;6&#39;）步骤前面所述。18 2.准备的1 1.3毫单体溶液中的电解质溶液<ol><li>制备的四正丁基六氟磷酸盐的0.1M库存电解质溶液，TBAPF 6，在乙腈，MeCN中。 <ol><li>放置的MeCN过度活化的3埃分子筛或K 2 CO 3，24小时，以除去外来的 H 2 O. </li><li>将TBAPF 6（0.969克，2.50毫摩尔）在25.00毫升火焰干燥的容量瓶中。 </li><li>过滤分子筛或K 2 CO从干乙腈3微粒，并把包含TBAPF的25.00毫升容量瓶<suB&gt; 6至体积。 </li></ol></li><li>放置1（0.0049克，5.2×10 -6摩尔）的干燥4英钱的小瓶或10毫升圆底烧瓶中，并添加4.00为0.1M TBAPF 6在MeCN原液的溶液中。 </li><li>转移3.5-4.0毫升1的红橙色着色电解液成3-隔室池的中央室，其中每个隔室通过中等孔率玻璃料分离。 </li><li>快速填充3-隔室电池的外部隔室，以相等的高度的中央室原液，与部分剩余的干的0.1M TBAPF 6的MeCN中，以防止泄漏到外室中。注意：时间是一个重要的因素，因为在不同的隔室的解决方案会慢慢混合并显著改变主隔室的浓度，如果溶剂的高度是不一样的。 </li></ol> 3. Electropolymerize 1对3毫米直径的玻璃Ÿ碳电极或1.0 平方厘米FTO电极<ol><li>准备隔氮/氩气排气管和电极。 <ol><li>切缝到每3个橡胶隔，引导薄聚四氟乙烯，PTFE，管通过狭缝。 </li><li>通过所述隔片的1滑动的Ag / 硝酸银参比电极，将参考电极/ PTFE管/隔膜在所述外室中的一个，并密封与 ​​隔垫的隔室。 </li><li>通过不同的隔膜代替铂线/ PTFE管/隔膜引导铂线/纱布反电极在所述外室中的一个，并密封与隔垫的隔室。如果狭缝不足够大或导线足够硬，以防止弯曲的金属丝，可以使用一个大口径针穿过隔膜以引导铂丝反电极。 </li><li>通过剩余的隔膜引导新鲜抛光3毫米玻碳电极，并把它使得电极是suspended在溶液中，或对于一个FTO滑动，引导连接到通过隔膜的鳄鱼夹的导线，然后夹紧用鳄鱼夹在FTO滑动，并确保浸没当滑动的导电面是垂直于对置电极。 <ol><li>之前插入玻碳电极：通过将氧化铝（0.5微米）上的润湿抛光垫抛光的玻璃碳，然后，将电极在一个8字形运动，持续30秒，同时保持电极垂直于所述垫 - 向抛光电极各方均匀-和冲洗任何剩余的氧化铝关闭了H 2Ø水喷瓶跟一个乙腈喷瓶冲洗。 </li><li>前夹紧在FTO滑动：环绕一个30×10mm的FTO滑动，使得所述滑动件的10×10mm的部分被暴露的中心部分的非导电卡普顿胶带几层。 </li><li>通过放置/保持在FTO幻灯片在POSIT收集在FTO幻灯片的UV-Vis光谱离子在已经预定以确保一致性分光计的光束路径。 </li></ol></li></ol></li><li>脱曝气在3-隔室电化学电池的解决方案。 <ol><li> Tygon管的一端连接至氮/氩气供给，将另一端连接到含有MeCN中的气体洗涤器。 </li><li>剪下另一块聚乙烯管，一端连接到流出乙腈冲氮气/氩气，另一端连接到4路分流。 </li><li>连接根PTFE管到分离器4的方式的3余下的连接。 </li><li>淹没根PTFE管进入溶液中的每个隔室的，并打开氮气/氩气的流量，使得所述溶液的快速鼓泡开始。 </li><li>继续脱气溶液5-10分钟，然后将聚四氟乙烯管只是溶液的表面上方，/氩离开，以保持惰性气体正压上的系统，并防止溶液氮气流Çonvection造成起泡。 </li></ol></li><li>进行电化学实验。 <ol><li>从电位在3-隔室单元的相应电极连接的电极。 </li><li>执行循环伏安法，CV实验使用以下参数：开关电位= 0V和-1.81伏;扫描/扫描速率= 100毫伏/秒;周期= 5的号码。 </li><li>当CV实验完成后，从聚合溶液中除去工作（玻璃碳或FTO）电极和轻轻地从吸液管或喷射瓶，以除去任何剩余的单体溶液冲洗用MeCN所述电极的表面上。 </li></ol></li></ol> 4.表面覆盖测定<ol><li>放置漂洗工作电极中的的0.1M TBAPF 6 / MeCN中新鲜制备的溶液中含有一对电极和一个参考电极（优选在electropolymerizatio使用的相同的参考电极的电化学电池N）。 </li><li>执行循环伏安法，CV实验使用以下参数：开关电位= 0和1.5伏;扫描/扫描速率= 100毫伏/秒;循环数= 15。 </li><li>整合在阳极和阴极峰的电荷的吸附electropolymer钌（III / II）的耦合，所述阳极和阴极的峰下平均化的电荷，并使用等式1确定表面覆盖。 </li><li>对于在FTO幻灯片：地点/保持在紫外可见样品支架，使得所述射束路径通过着色膜的前面在预定位置在FTO滑动。在FTO幻灯片可以是湿法或干法，但在相同的条件下做比较作为空白谱下收集。 </li><li>减去用于收集该特定幻灯片的FTO光谱得到的频谱之前从薄膜上的FTO的频谱，以便产生的吸收光谱为电影本身电解。 </li></ol>

<ol>
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Electroanal. Chem. Interfacial Electrochem. 115, 65-74 (1980).</li><li>Laviron, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+in+the+case+of+diffusionless+electrochemical+systems.">General expression of the linear potential sweep voltammogram in the case of diffusionless electrochemical systems.</a> J. Electroanal. Chem. 101, 19-28 (1979).</li><li>Ratcliff, E. L., Jenkins, J. L., Nebesny, K., Armstrong, N. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposited,+&#34;Textured&#34;+Poly(3-hexyl-thiophene)+(e-P3HT)+Films+for+Photovoltaic+Applications.">Electrodeposited, &#34;Textured&#34; Poly(3-hexyl-thiophene) (e-P3HT) Films for Photovoltaic Applications.</a> Chemistry of Materials. 20, 5796-5806 (2008).</li></ol>

No conflicts of interest declared.

电化学提供了一个大范围的可控变量是不常见的其他技术。除了 ​​标准的反应变量，如试剂（单体）浓度，温度，溶剂等 ，电解可以另外通过共同的电化学方法电化学实验参数控制。 CV扫描速率，切换电位，和循环次数影响electropolymers的沉积。例如，作为循环通过配体还原波的数量增加，所以也是表面覆盖。在这里提出的范围内，是线性的相对于执行的周期数（ 见表1）。 ...

电解是利用施加的电势以引发单体的前体的聚合直接在电极的表面上并已被利用来生产薄电活性和/或光化学活性多吡啶薄膜上的电极和半导体的表面上。1-4电催化的聚合技术， 5-10电子转移，11，12光化学，13-16电致变色，17和配位化学18已经研究了电聚合膜。这项技术最早是在北卡罗莱纳州的乙烯基3，5，7，8，11-15，19，20和吡咯6,9的电化学一个迈耶-穆雷合作大学，21-24衍生我TAL络合物对各种导电衬底。 图1给出了一些，当配位到金属配合物，已产生electropolymers共同吡啶基配体。在还原性电解，含乙烯基化合物的电解时发生缀合的乙烯基吡啶配体的减少，而与吡咯官能配位体，电解是由吡咯部分的氧化发起的，从而导致氧化电解（ 图2）。电解技术，用于直接连接几乎任何过渡金属配合物的任何电极上设置的一般化方法的目的开发的。该方法的多样性打开大门，electropolymer修饰电极的大量调查。 而相比之下，其他附接策略，这涉及直接接合到电极，电解提供了副antage不需要电极表面预修饰。因此它可以应用无论表面组成或形态4，10，25，以任何数量的导电基板，26这种多功能性是变化的物理性质的聚合物长度的增长的结果;所述单体可溶于电解液而是作为发生聚合和交联rigidifies薄膜，沉淀和物理吸附在电极表面发生（ 图3）。27 相比氧化物表面结合的羧酸酯，它们是不稳定的氧化物表面的水，或膦酸酯衍生的复合物，它们是不稳定的，在升高的pH值的，在太阳能燃料研究常用，这些界面的电极的聚合物膜结构提供了稳定性的额外的好处在各种媒体，包括有机溶剂和水在​​大的pH范围（0-14）。28-30电聚合还可以存大范围明显的表面覆盖范围，从亚单层至数十或数百当量单层，而羧酸盐或磷酸盐衍生复合接口结构局限于单层表面覆盖度的电影。 虽然任何数量的乙烯基或含吡咯吡啶基和聚吡啶化合物能够聚合的，使用[Ru II（PhTpy）（5,5&#39;- dvbpy）（MeCN中）]（PF 6）2，（1; PhTpy是4&#39;-苯基-2,2&#39;：6&#39;，2&#39;&#39; -三联吡啶; 5,5&#39;- dvbpy是5,5&#39;-二乙烯基-2,2&#39;-联吡啶; 图4）将被用作模型复杂证明还原电解上玻璃碳和氟掺杂的氧化锡，FTO，本报告中的电极1是现代electropolymer前体具有潜在的电的应用的一个例子，并且由于其金属对利GAND电荷转移，MLCT，吸收光谱躺在光光谱的可见光区，可以用UV-Vis光谱。18，30请注意，某些结果呈现此处为1已经发表在稍微修改的形式。18调查

<table border="0" cellpadding="0" cellspacing="0" width="652">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:384px;">Name of Reagent/ Equipment</td>
			<td style="width:108px;">Company</td>
			<td style="width:160px;">Catalog Number</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Tetrabutylammonium hexafluorophosphate for electrochemical analysis, &#8805;99.0%,&#160;</td>
			<td>Sigma-Aldrich</td>
			<td>86879-25G</td>
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			<td height="20" style="height:20px;width:384px;">Acetonitrile&#160;(Optima LC/MS), Fisher Chemical</td>
			<td>Fisher Scientific</td>
			<td>A955-4</td>
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		<tr height="20">
			<td height="20" style="height:20px;">3 mm dia. Glassy Carbon Working Electrode</td>
			<td>CH Instruments</td>
			<td>CH104</td>
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		<tr height="20">
			<td height="20" style="height:20px;">Non-Aqueous Ag/Ag+ Reference Electrode w/ porous Teflon Tip</td>
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			<td>CHI112</td>
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			<td height="20" style="height:20px;">Platinum&#160;gauze</td>
			<td>Alfa Aesar</td>
			<td>AA10282FF&#160;</td>
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		<tr height="20">
			<td height="20" style="height:20px;">Electrode Polishing Kit</td>
			<td>CH Instruments</td>
			<td>CHI120</td>
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			<td height="20" style="height:20px;width:384px;">Cole-Parmer KAPTON TAPE&#160;1/2IN X 36 YD</td>
			<td>Fisher Scientific</td>
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			<td height="20" style="height:20px;width:384px;">Fisherbrand Polypropylene Tubing&#160;4-Way&#160;Connectors</td>
			<td>Fisher Scientific</td>
			<td>15-315-32B</td>
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			<td height="20" style="height:20px;">500mL Bottle, Gas Washing, Tall Form, Coarse Frit</td>
			<td>Chemglass</td>
			<td>CG-1114-15</td>
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			<td height="20" style="height:20px;">3 compartment H-Cell for electrochemistry</td>
			<td colspan="2">Custom made H-cell with 3 compartments</td>
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</table>

reductive electropolymerization of a vinyl-containing poly-pyridyl complex on glassy carbon and fluorine-doped tin oxide electrodes

可控电极表面改性是在许多领域，特别是那些与太阳能电池的燃料的应用是重要的。电解是通过利用施加的电势来启动，在亥姆霍兹层基板的聚合镀层在电极的表面上的聚合物膜的一个表面改性技术。这种有用的技术，最早是由美国北卡罗来纳大学教堂山分校在20世纪80年代初穆雷梅耶尔合作建立并用来研究含无机复合物作为单体基材薄膜众多的物理现象。在这里，我们突出显示用无机复合涂层的电极的程序通过执行含乙烯基的聚吡啶基络合物的还原性电解到玻璃碳和氟掺杂氧化锡涂层的电极。电化学电池配置和故障排除程序的建议都包括在内。虽然不是ê这里xplicitly描述的，含吡咯的化合物的氧化电聚合遵循类似程序，以乙烯基类还原性电解，但远不如敏感为氧气和水。

Electropolymer增长遵守规定的CV实验（协议文本STEP 3.3.2）的进展情况时，最容易识别。 图5体现在0.071厘米2（3毫米直径）electropolymer增长，1玻碳电极。在实验的第一周期产生一个伏安大致类似于该预计为类似浓度（ 图5，黑色迹线），但的钌溶液在连续循环，通过第 1 次和第2 次的配体为本还原波，日益增强的电流是观察到的（ ...

Watch this Scientific Journal Video about Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes at JoVE.com

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

在玻碳和氟掺杂的氧化锡电极的含乙烯基聚吡啶基复合还原电聚合

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

reductive-electropolymerization-vinyl-containing-poly-pyridyl-complex

Research

JoVE Journal

Chemistry

11.7K 次观看.  Virginia Military Institute. A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization. 

视频: Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Improved In-gel Reductive &#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of biological samples. Similar approaches, that would allow in-depth analysis of the glycans carried by glycoproteins resolved by SDS-PAGE, require special considerations in order to maximize recovery and sensitivity when using mass spectrometry (MS) as the detection method. A major hurdle to be overcome in achieving high-quality data is the removal of gel-derived contaminants that interfere with MS analysis. The sample workflow presented here is robust, efficient, and eliminates the need for in-line HPLC clean-up prior to MS. Gel pieces containing target proteins are washed in acetonitrile, water, and ethyl acetate to remove contaminants, including polymeric acrylamide fragments. O-linked glycans are released from target proteins by in-gel reductive &#946;-elimination and recovered through robust, simple clean-up procedures. An advantage of this workflow is that it improves sensitivity for detecting and characterizing sulfated glycans. These procedures produce an efficient separation of sulfated permethylated glycans from non-sulfated (sialylated and neutral) permethylated glycans by a rapid phase-partition prior to MS analysis, and thereby enhance glycomic and sulfoglycomic analyses of glycoproteins resolved by SDS-PAGE.

Improved In-gel Reductive &amp;#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

In order to comprehensively explore the diversity of O-linked glycans, a new procedure for in-gel reductive &#946;-elimination, combined with permethylation and a rapid phase-partition method, is applied to the analysis of O-linked glycans directly released from glycoproteins resolved by SDS-PAGE and amenable to subsequent glycomic analysis by mass spectrometry.

改善凝胶还原β-消除综合O连接和磺基糖组学质谱

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of ...

科研

化学

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

原子定义模板复合氧化物薄膜的外延生长

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

表面修饰碳纳米管通过土柱运输

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

铱氧化物纳米颗粒对硒化镉硫化镉@纳米棒光化学氧化增长

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

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 ...

Investigations on the Ga(III) Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) complex and protocols for the preparation of its novel non-radioactive, i.e., natural Ga(III) as well as radioactive 68Ga complex. The ligand as well as the Ga(III) complex were characterized by nuclear magnetic resonance (NMR) spectroscopy, mass spectrometry and elemental analysis. 68Ga was obtained by a standard elution method from a 68Ge/68Ga generator. Experiments to evaluate the 68Ga-labeling efficiency of EOB-DTPA at pH 3.8&#8211;4.0 were performed. Established analysis techniques radio TLC (thin layer chromatography) and radio HPLC (high performance liquid chromatography) were used to determine the radiochemical purity of the tracer. As a first investigation of the 68Ga tracers&#39; lipophilicity the n-octanol/water distribution coefficient of 68Ga species present in a pH 7.4 solution was determined by an extraction method. In vitro stability measurements of the tracer in various media at physiological pH were performed, revealing different rates of decomposition.

Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

A procedure for the isolation of EOB-DTPA and subsequent complexation with natural Ga(III) and 68Ga is presented herein, as well as a thorough analysis of all compounds and investigations on labeling efficiency, in vitro stability and the n-octanol/water distribution coefficient of the radiolabeled complex.

在EOB-DTPA和镓（三）复杂的调查其<sup&gt; 68</sup&gt;嘎放射性标记模拟

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

用聚苯乙烯接枝多壁纳米碳纳米管使自组装和各向异性斑块

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

电化学阻抗谱作为电化学速率常数估计的一种工具

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

溶剂热合成 MIL-96 和 UiO-66-NH2在纤维垫上原子层沉积金属氧化物涂层上的合成

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Negative Additive Manufacturing of Complex Shaped Boron Carbides

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for high wear, high hardness, and lightweight material applications such as armors. To overcome this challenge, negative additive manufacturing (AM) is employed to produce complex geometries of boron carbides at various length scales. Negative AM first involves gelcasting a suspension into a 3D-printed plastic mold. The mold is then dissolved away, leaving behind a green body as a negative copy. Resorcinol-formaldehyde (RF) is used as a novel gelling agent because unlike traditional hydrogels, there is little to no shrinkage, which allows for extremely complex molds to be used. Furthermore, this gelling agent can be pyrolyzed to leave behind ~50 wt% carbon, which is a highly effective sintering aid for B4C. Due to this highly homogenous distribution of in situ carbon within the B4C matrix, less than 2% porosity can be achieved after sintering. This protocol highlights in detail the methodology for creating near fully dense boron carbide parts with highly complex geometries.

A method called negative additive manufacturing is used to produce near fully dense complex shaped boron carbide parts of various length scales. This technique is possible via the formulation of a novel suspension involving resorcinol-formaldehyde as a unique gelling agent that leaves behind a homogenous carbon sintering aid after pyrolysis.

复合型碳化硼的负添加剂制造

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for ...