作者承认空军研究实验室的下UES分包合同＃S-932-19-MR002的支持。作者进一步确认设备的支持来自纽约州研究生研究和教学计划（GRTI / GR15）。

1.预分析样品制备<ol><li>分离油墨从车辆功能性颗粒：离心<ol><li>基于初始油墨配方，计算需要多少墨水样品需要获得最小2.0克的颗粒沉淀物。例如，如果墨是10体积％的陶瓷和陶瓷的密度是6.67克/厘米3，则最小为3.0毫升墨水的需要，以产生2.0克沉积物。 </li><li>吸管的至少最低要求的墨量到离心管中。离心管的选择应根据所需的油墨量和管材料的惰性至油墨溶剂来制备。 </li><li>将管离心机。离心机和旋转速率的选择将由以沉淀墨粒子所需的重力决定。一个标准的实验室离心机像SORVALL ST16离心机与TX-200水平转头通常是足够的。 </li><li>计划离心机旋转墨在旋转RA德和必要的时间，以产生一清晰的上清液。对于这里使用的离心机，典型的费率和时间是3000 - 4000转分钟的30分钟和90。到达正确的转速和必需的时间以沉淀的墨水可能需要反复试验，因为相同的平均颗粒尺寸的连油墨可具有不同的粒度分布。 </li></ol></li><li>分离后的样品处理：去除上清液，样品洗涤，干燥<ol><li>一旦上层清液已经实现，从离心机取出离心管中。 </li><li>滗析出上清液，并保存以备将来可能分析带盖玻璃样品瓶。功能性微粒是现在残存的离心管中。 </li><li>倾析后，将未加帽的离心管在纸巾上倒置，并允许额外的上清滴出，持续1分钟。 </li><li>从纸巾取出管并通过向冲洗沉淀的颗粒管大约2毫升在油墨制剂中所用的相同组成的新鲜溶剂。请注意，此溶剂将只摸沉淀在离心管中颗粒的最上面的层。滗出溶剂。重复漂洗循环三次。 </li><li>最终漂洗周期之后，将未加帽的离心管在纸巾上倒置，并允许额外的溶剂滴出约5分钟。 </li><li>使用一个薄的金属刮刀从离心管的底部除去沉积物，并蔓延到一个干净的，干燥的表玻璃。使用不起毛的非研磨棉签或干净的铲尖从小勺除去多余的颗粒。 </li><li>将表面皿置于50℃的烘箱，并允许该颗粒干燥24小时。炉子的温度应保持在相对低，以最小化降解吸附物种的可能性。需要用于干燥颗粒中的时间将取决于该溶剂的蒸气压。 24小时是典型的，但是结果通常是不敏感的等待时间短至12小时和长达3周。 </li></ol></li></ol> 2.漫反射红外光谱测量<ol><li>准备红外光谱仪：调整配件，清洗室<ol><li>打开红外光谱仪。 </li><li>为了准备漫反射红外光谱测量，将漫反射采样附件进入红外光谱仪的采样舱。红外光谱仪可以是任何傅里叶变换能够与漫反射采样装置接口的红外光谱仪。使用Shimadzu IR威望21光谱仪接口与派克科技EasiDiff配件被用于该协议。对于大多数的油墨颗粒，一个标准的氘，L-丙氨酸掺杂三甘氨酸硫酸盐（DLATGS）检测器提供了足够的灵敏度进行测定。液氮冷却的碲镉汞（MCT）Detector提供一个四到灵敏度提高十倍，但是这通常不是必要的用于识别墨粒子表面吸附物。 </li><li>漫反射率采样附件对齐按照制造商的说明。 </li></ol></li><li>调整后，关闭红外采样舱，并开始用氮气或无二氧化碳排放，空气干燥（10升/分钟清除率）清洗。一个标准的帕克Balston的FT-IR吹扫气体发生器提供空气与低于1ppm水和CO 2。的必要，以获得一个稳定的水和CO 2的分类室吹扫时间的量将依赖于样本室配置和湿度在实验室。必要的吹扫时间可通过实验比较的背景光谱采取在1或2分钟的间隔，并评估水的强度和CO 2频带作为时间的函数来确定。 </li><li>准备样品漫反射红外光谱MEASurement <ol><li>获得以下样品制备附件：小（35毫米）玛瑙研钵和杵，小金属刮刀，直刀片，以及两个漫反射红外线的样品杯。擦拭干净，用乙醇配件，然后用丙酮，并允许他们在50℃的烘箱中干燥10分钟。 </li><li>从烤箱中取出清洁，干燥的样品制备配件，将它们放在一个大的Kimwipe，并让他们冷却至室温。 </li><li>同时将样品制备配件冷却，从炉中取出干燥的油墨颗粒，并使用一个分析天平来测量0.025克颗粒样品。离开样品坐在分析天平。 </li><li>返回样品制备配件，倒0.5克KBr压入玛瑙研钵中。始终使用溴化钾售价为红外应用。溴化钾（The​​rmo Scientific）进行的预测个体0.5克包被推荐的，因为它们最小化称量时间和吸湿溴化钾暴露于ambie新台币水蒸气。研磨KBr压到一个统一的外观，通常是1分钟的连续手工研磨的。 </li><li>完全填满漫反射红外线取样杯与地面溴化钾粉末之一。轻轻按下与杵的钝端的粉，顶过采样杯溴化钾。 </li><li>使用剃刀刀片的侧弄平溴化钾的顶部在样品杯中。此填充和平坦化样本是参考或背景。 </li><li>处理任何溴化钾留在砂浆，并擦拭干净。 </li><li>打开溴化钾粉末的新0.5克分组（或者添加0.5克溴化钾粉末），并倒入砂浆。 </li><li>添加预先称重0.025克墨粒子的0.5克溴化钾的，和研磨带杵以形成均匀的粉末，通常为1分钟连续手工研磨。墨粒子与溴化钾该比值提供了测量在5％（重量）的样品。这是标准的范围内（1 - 10重量％），但也可以上下调整取决于ön个样本的吸收率和信号强度。 </li><li>按照步骤2.3.5和2.3.6创建充满颗粒/溴化钾混合物样品杯。 </li></ol></li><li>红外光谱检测<ol><li>放置参考和样品杯插入支架，和保持器放置到漫反射红外光谱采样附件。保持器定位使得包含背景杯（纯溴化钾）材料暴露于红外辐射。 </li><li>关闭红外采样隔室，并允许隔室吹扫5分钟。此吹扫时间可根据所需的时间量确定为必要的，在步骤2.2进行调整。 </li><li> 5分钟后清洗的，得到在所关心的区域中的背景的红外光谱。扫描的次数应设置的信号最大化信噪比，同时尽量减少测量时间。 128扫描在4 -1的分辨率通常是足够的。 </li><li>的背景和经过ð扫描完成时，打开红外样品室和移动包含颗粒/溴化钾混合物使得它现在暴露于红外辐射的杯子。 </li><li>重复步骤2.4.2和2.4.3得到的粒子/溴化钾混合物的光谱。 </li></ol></li></ol>

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的两个关键因素的产生高品质的红外光谱使用此过程是：1）最小化水的污染的绝对量和在样品和参比杯之间的水的污染的量的差异;和2）创建样本和参照杯具有均匀平坦层和类似溴化钾晶粒尺寸。这两个因素都受到特别注意在2.3节所列的样品制备程序来实现的。 为了最大限度地减少水的污染的总量，并保持水的污染的参比和样品相同，有必要尽量减少时间，该吸湿溴化钾是?...

添加剂制造近来成为一个有前途的技术，一切从陶瓷半导体制造医疗器械1。作为添加剂制造的应用扩大到印刷陶瓷，金属氧化物，和金属零件，需要制定专门功能性油墨产生。如何制定所需的功能性油墨的问题涉及到一个根本性的问题，表面和胶体科学：什么是由胶体粒子分散体是稳定的防止聚集的机制？广泛地说，稳定化需要，从而防止颗粒（和因此聚合）的附近的方式或者通过库仑斥力（静电稳定化），由聚合物缠结（空间稳定）的熵惩罚，或由库仑的组合的颗粒表面的变形和熵力（电空间稳定）2。为了实现任何的这些机制稳定化，通常需要通过附着聚合物或较短链的官能团进行修改的粒子表面的化学反应。因此，稳定的功能性油墨的合理配方要求我们知道给定的化学添加剂是否附着到颗粒表面和什么化学基团附着到颗粒表面。 在这个协议中提出的方法的目的是要证明在功能性油墨吸附在颗粒表面的化学物种的快速鉴定。这个目标是从表面和胶体科学家科学家和感兴趣印刷陶瓷，金属氧化物和金属设备工程师的范围广泛的实践活性的专门任务官能油墨制剂跃迁特别重要。实现这一目标，需要设计一种克服表征不透明，高固体负载分散体的挑战的实验。它还需要鉴别通道之间emical物种中存在的分散体，但不吸附在从那些实际吸附的颗粒。它还需要被化学吸附在从那些弱物理吸附的颗粒的那些物种之间进行区分。在这个实验方案，我们提出利用漫反射红外光谱仪对分散剂附着在功能性油墨的特性。漫反射红外光谱测量如下必要区分吸附物质从那些仅仅存在于分散体中的分析前的样品制备技术。 多种方法目前用于洞察化学油墨组分和胶态分散颗粒之间的相互作用的性质。一些这些方法是间接的探针，其中测得特性被假定为关联与表面官能化。例如，改变泥浆流变性或沉淀 - [R阿泰被推定与相关吸附表面改性剂3。粒径分布，作为其特征在于通过动态光散射（DLS），和ζ电位，为特征的电泳迁移率，提供深入了解聚合物或物种的表面电荷4,5的吸附。同样地，采样的质量损失为探测由热重量分析（TGA）涉及解吸物质的存在和被吸附物和粒子6之间的相互作用的强度。从上面提到的间接探针的信息表明改变表面化学性质，但它们不提供直接洞察吸附物种的身份，或它的吸附机理。直接洞察为功能性油墨，其中，大量的部件都存在于分散体特别重要。为了提供更详细的分子水平信息，X射线光电子能谱（XPS）7，13 C核磁振（NMR）4,6，和红外光谱8-12已探索。这三个选项中，红外光谱法是特别有前途。在比较13 C-NMR，红外光谱不需要油墨，分析纯溶剂进行配制，以防止测量13过程中的干扰。相比于X射线光电子能谱，标准红外光谱可以在环境压力下进行，避免了需要在测量过程中超高真空条件。 有文献先例利用红外光谱探测胶态分散陶瓷，金属氧化物，和金属纳米粒子之间的相互作用。这些作品可以分离成尝试使用衰减全反射红外（ATR-IR）的9到测量原位界面化学，并尝试使用固体采样8以测量界面化学易地 。 W¯¯往往微不足道有优势现场测量，出现由于需要进行光谱操作的不确定性使该方法难以用于多组分的油墨，其中有溶剂和多种聚合物组分。因此，该协议侧重于固体取样和易地测量。所有的固体采样方法需要在那里的固体通过从溶剂中分离出的颗粒而得到的前处理步骤，并在红外线测量上的固体颗粒进行的分析步骤。方法之间的不同是在样品前处理的选择和在用于固体的红外分析实验技术的选择。在历史上，传统的方式来使用红外光谱来分析固体含量为研磨少量用溴化钾（KBr压）粉末固体样品的（&lt;1％），然后经受混合物以高压烧结。其结果是透明KBr压片。该公关ocedure已成功地尝试与来自官能化聚乙烯胺10氧化锆纳米粒子的水性悬浮液，用脂肪酸单层钴纳米颗粒7的粉末，并与对Fe 3 O 4纳米颗粒14儿茶酚衍生的分散剂。尽管检测吸附的分散剂的溴化钾造粒技术的这些成功的应用，漫反射红外光谱提供了几个优点。一个优点是简化了样品制备。在对比溴化钾造粒，在漫反射固体样品可以简单地用手工研磨。不存在烧结步骤作为本身被装入样品杯和漫散射的红外光进行测量的粉末。漫反射在KBr压造粒的另一优点是增加的表面灵敏度15。在表面灵敏度的增加是对于本申请特别有用，其中，CRI蒂卡尔问题是存在和吸附物的性质的纳米颗粒的表面上。 在已经使用了漫反射采样技术来探测在胶态分散的样品的化学物质的吸附作品，一次差值出现在从液体介质中分离出纳米颗粒的方法。这个步骤是关键的，因为如果没有分离，这将是不可能区分从分散剂简单地溶解在液体介质中特殊吸附分散剂。在几个实例中，分离的方法，没有从实验方案12,16,17明显。当指定时，最常采用的方法包括重力分离。的理由是，陶瓷，金属氧化物，以及金属纳米颗粒的所有比周围介质更加密集。当他们定居，他们将拖累他们只特异性吸附物种。化学物质不与部分交互icles将留在溶液中。虽然可能分散在正常重力18随手解决，稳定的喷墨油墨不宜observably解决在不到一年的时间。因此，优选采用离心预分析分离的方法。这已被证明在分散剂吸附的几项研究对玻璃微粒19,20，在氧化铝上的8分散剂粘合剂吸附和CuO 11的阴离子分散剂官能化。最近，我们用它来 ​​评估的脂肪酸中使用的固体氧化物燃料电池层21的喷墨和气溶胶喷射印刷的非水氧化镍分散体结合的机制。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>FTIR bench</td>
			<td>Shimadzu Scientific Instruments</td>
			<td>IR_Prestige 21 used in this work; in 2013 IR-Tracer 100 model replaced Prestige-21</td>
			<td>Any research grade FTIR with purgable sample compartment is acceptable</td>
		</tr>
		<tr>
			<td>Purge gas generator for sample compartment</td>
			<td>Parker Balston</td>
			<td>74-5041NA Lab Gas Generator</td>
			<td>Provides air with less than 1ppm CO2 and water; also possible to purge compartment with N2 tank</td>
		</tr>
		<tr>
			<td>Diffuse Reflectance Infrared Accessory</td>
			<td>Pike Technologies</td>
			<td>042-10XX</td>
			<td>Includes sample preparation kit and mortar and pestle (these can also be purchased separately, described below)</td>
		</tr>
		<tr>
			<td>Diffuse Reflectance Sample Preparation kit</td>
			<td>Pike Technologies</td>
			<td>042-3040</td>
			<td>Includes sample holder cups, spatulas, alignment mirror, mirror brush, razor blades</td>
		</tr>
		<tr>
			<td>Agate mortar and pestle</td>
			<td>Pike Technologies</td>
			<td>161-5035</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>ThermoScientific</td>
			<td>Sorvall ST16</td>
			<td>Most benchtop centrifuges capable of ~ 5000 rpm will be acceptable</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Consumables</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Item</td>
			<td>Company</td>
			<td>Catalog #</td>
			<td>Comments/Description</td>
		</tr>
		<tr>
			<td>Centrifuge tubes</td>
			<td>Evergreen Scientific</td>
			<td>222-2470-G8K</td>
			<td>Any centrifuge tube of compatible size and material is acceptable</td>
		</tr>
		<tr>
			<td>KBr powder packets</td>
			<td>ThermoScientific</td>
			<td>50-465-317</td>
			<td>Also possible to use alternative KBr supplier</td>
		</tr>
	</tbody>
</table>

diffuse reflectance infrared spectroscopic identification of dispersant/particle bonding mechanisms in functional inks

In additive manufacturing, or 3D printing, material is deposited drop by drop, to create micron to macroscale layers. A typical inkjet ink is a colloidal dispersion containing approximately ten components including solvent, the nano to micron scale particles which will comprise the printed layer, polymeric dispersants to stabilize the particles, and polymers to tune layer strength, surface tension and viscosity. To rationally and efficiently formulate such an ink, it is crucial to know how the components interact. Specifically, which polymers bond to the particle surfaces and how are they attached? Answering this question requires an experimental procedure that discriminates between polymer adsorbed on the particles and free polymer. Further, the method must provide details about how the functional groups of the polymer interact with the particle. In this protocol, we show how to employ centrifugation to separate particles with adsorbed polymer from the rest of the ink, prepare the separated samples for spectroscopic measurement, and use Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) for accurate determination of dispersant/particle bonding mechanisms. A significant advantage of this methodology is that it provides high level mechanistic detail using only simple, commonly available laboratory equipment. This makes crucial data available to almost any formulation laboratory. The method is most useful for inks composed of metal, ceramic, and metal oxide particles in the range of 100 nm or greater. Because of the density and particle size of these inks, they are readily separable with centrifugation. Further, the spectroscopic signatures of such particles are easy to distinguish from absorbed polymer. The primary limitation of this technique is that the spectroscopy is performed ex-situ on the separated and dried particles as opposed to the particles in dispersion. However, results from attenuated total reflectance spectra of the wet separated particles provide evidence for the validity of the DRIFTS measurement.

在这个协议中所述的实验步骤已应用于洞察的NiO颗粒稳定的机制中用于打印的固体氧化物燃料电池的阳极的油墨。这种油墨是氧化镍粒子在2-丁醇，α-萜品醇，和一系列分散剂和粘合剂22中的分散体。代表性的结果示此处的NiO在2-丁醇的简化分散用油酸分散剂。在图1A中，我们表明生漫反射红外光谱数据。为了解释该数据，有必要比较之前分散体（ 图1B）从分散到?...

Watch this Scientific Journal Video about Diffuse Reflectance Infrared Spectroscopic Identification of Dispersant/Particle Bonding Mechanisms in Functional Inks at JoVE.com

Diffuse Reflectance Infrared Spectroscopic Identification of Dispersant/Particle Bonding Mechanisms in Functional Inks

Formulation of stable, functional inks is critical to expanding the applications of additive manufacturing. In turn, knowledge of the mechanisms of dispersant/particle bonding is required for effective ink formulation. Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) is presented as a simple, inexpensive way to gain insight into these mechanisms.

弥漫分散剂/粒子绑定机制反射红外光谱鉴定功能性油墨

In additive manufacturing, or 3D printing, material is deposited drop by drop, to create micron to macroscale layers.  A typical inkjet ink is a colloidal ...

diffuse-reflectance-infrared-spectroscopic-identification

Research

JoVE Journal

Chemistry

13.6K 次观看.  New York City College of Technology, City University of New York (CUNY). Formulation of stable, functional inks is critical to expanding the applications of additive manufacturing. In turn, knowledge of the mechanisms of dispersant/particle bonding is required for effective ink formulation. Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) is presented as a simple, inexpensive way to gain insight into these mechanisms.

视频: Diffuse Reflectance Infrared Spectroscopic Identification of Dispersant/Particle Bonding Mechanisms in Functional Inks

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

层 - 层的合成和独立式共轭微孔聚合物纳米薄膜的转移

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

科研

化学

A Filter-based Surface Enhanced Raman Spectroscopic Assay for Rapid Detection of Chemical Contaminants

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be applied to the detection of various chemical contaminants. Silver nanoparticles (Ag NPs) are synthesized via reduction of silver nitrate by sodium citrate. Then the NPs are aggregated by sodium chloride to form nanoclusters that could be trapped in the pores of the filter membrane. A syringe is connected to the filter holder, with a filter membrane inside. By loading the nanoclusters into the syringe and passing through the membrane, the liquid goes through the membrane but not the nanoclusters, forming a SERS-active membrane. When testing the analyte, the liquid sample is loaded into the syringe and flowed through the Ag NPs coated membrane. The analyte binds and concentrates on the Ag NPs coated membrane. Then the membrane is detached from the filter holder, air dried and measured by a Raman instrument. Here we present the study of the volume effect of Ag NPs and sample on the detection sensitivity as well as the detection of 10 ppb ferbam and 1 ppm ampicillin using the developed assay.

A procedure for fabrication and performing the filter-based surface enhanced Raman spectroscopic (SERS) assay for the detection of chemical contaminants (i.e., pesticide ferbam and antibiotic ampicillin) is presented.

基于过滤器的表面增强拉曼光谱检测方法的化学污染物快速检测

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be ...

Construction of Models for Nondestructive Prediction of Ingredient Contents in Blueberries by Near-infrared Spectroscopy Based on HPLC Measurements

Nondestructive prediction of ingredient contents of farm products is useful to ship and sell the products with guaranteed qualities. Here, near-infrared spectroscopy is used to predict nondestructively total sugar, total organic acid, and total anthocyanin content in each blueberry. The technique is expected to enable the selection of only delicious blueberries from all harvested ones. The near-infrared absorption spectra of blueberries are measured with the diffuse reflectance mode at the positions not on the calyx. The ingredient contents of a blueberry determined by high-performance liquid chromatography are used to construct models to predict the ingredient contents from observed spectra. Partial least squares regression is used for the construction of the models. It is necessary to properly select the pretreatments for the observed spectra and the wavelength regions of the spectra used for analyses. Validations are necessary for the constructed models to confirm that the ingredient contents are predicted with practical accuracies. Here we present a protocol to construct and validate the models for nondestructive prediction of ingredient contents in blueberries by near-infrared spectroscopy.

We present here a protocol to construct and validate models for nondestructive prediction of total sugar, total organic acid, and total anthocyanin content in individual blueberries by near-infrared spectroscopy.

基于HPLC测量通过近红外光谱对在蓝莓成分的含量无损预测模型的构建

Nondestructive prediction of ingredient contents of farm products is useful to ship and sell the products with guaranteed qualities. Here, near-infrared ...

Site Directed Spin Labeling and EPR Spectroscopic Studies of Pentameric Ligand-Gated Ion Channels

Ion channel gating is a stimulus-driven orchestration of protein motions that leads to transitions between closed, open, and desensitized states. Fundamental to these transitions is the intrinsic flexibility of the protein, which is critically modulated by membrane lipid-composition. To better understand the structural basis of channel function, it is necessary to study protein dynamics in a physiological membrane environment. Electron Paramagnetic Resonance (EPR) spectroscopy is an important tool to characterize conformational transitions between functional states. In comparison to NMR and X-ray crystallography, the information obtained from EPR is intrinsically of lower resolution. However, unlike in other techniques, in EPR there is no upper-limit to the molecular weight of the protein, the sample requirements are significantly lower, and more importantly the protein is not constrained by the crystal lattice forces. Therefore, EPR is uniquely suited for studying large protein complexes and proteins in reconstituted systems. In this article, we will discuss general protocols for site-directed spin labeling and membrane reconstitution using a prokaryotic proton-gated pentameric Ligand-Gated Ion Channel (pLGIC) from Gloeobacter violaceus (GLIC) as an example. A combination of steady-state Continuous Wave (CW) and Pulsed (Double Electron Electron Resonance-DEER) EPR approaches will be described that will enable a complete quantitative characterization of channel dynamics.

This article describes methods for site-directed spin labeling and reconstitution of pentameric ligand-gated channels for Electron Paramagnetic Resonance studies. This protocol can be adapted for any membrane protein. The reconstitution method described here can also be used for patch-clamp measurements of macroscopic and single-channel currents in a defined lipid system.

定点自旋标记和五聚体配体门控离子通道的EPR光谱研究

Ion channel gating is a stimulus-driven orchestration of protein motions that leads to transitions between closed, open, and desensitized states. ...

From Molecules to Materials: Engineering New Ionic Liquid Crystals Through Halogen Bonding

Herein, we demonstrate that a bottom-up approach, based on halogen bonding (XB), can be successfully applied for the design of a new type of ionic liquid crystals (ILCs). Taking advantages of the high specificity of XB for haloperfluorocarbons and the ability of anions to act as XB-acceptors, we obtained supramolecular complexes based on 1-alkyl-3-methylimidazolium iodides and iodoperfluorocarbons, overcoming the well-known immiscibility between hydrocarbons (HCs) and perfluorocarbons (PFCs). The high directionality of the XB combined with the fluorophobic effect, allowed us to obtain enantiotropic liquid crystals where a rigid, non-aromatic, XB supramolecular anion acts as mesogenic core.
X-ray structure analysis of the complex between 1-ethyl-3-methylimidazolium iodide and iodoperfluorooctane showed the presence of a layered structure, which is a manifestation of the well-known tendency to segregation of perfluoroalkyl chains. This is consistent with the observation of smectic mesophases. Moreover, all the reported complexes melt below 100 &#176;C, and most are mesomorphic even at room temperature, despite that the starting materials were non-mesomorphic in nature.
The supramolecular strategy reported here provides new design principles for mesogen design allowing a totally new class of functional materials.

A protocol for the synthesis of a new type of mesogens, based on the halogen-bonded supramolecular anion [CnF2n+1-I&#183;&#183;&#183;I&#183;&#183;&#183;I-CnF2n+1]&#8722;, is reported.

从分子到材料: 通过卤素键合工程新的离子液体晶体

Herein, we demonstrate that a bottom-up approach, based on halogen bonding (XB), can be successfully applied for the design of a new type of ionic liquid ...

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical photocatalytic structures. However, the influence of such chemical bonding on the optical and surface properties of the photocatalyst and thus its photocatalytic activity/reaction selectivity behavior has not been systematically studied. In this investigation, TiO2 has been supported on the surface of SiO2 by means of two different methods: (i) by the in situ formation of TiO2 in the presence of sand quartz via a sol-gel method employing tetrabutyl orthotitanium (TBOT); and (ii) by binding the commercial TiO2 powder to quartz on a surface silica gel layer formed from the reaction of quartz with tetraethylorthosilicate (TEOS). For comparison, TiO2 nanoparticles were also deposited on the surfaces of a more reactive SiO2 prepared by a hydrolysis-controlled sol-gel technique as well as through a sol-gel route from TiO2 and SiO2 precursors. The combination of TiO2 and SiO2, through interfacial Ti-O-Si bonds, was confirmed by FTIR spectroscopy and the photocatalytic activities of the obtained composites were tested for photocatalytic degradation of NO according to the ISO standard method (ISO 22197&#8722;1). The electron microscope images of the obtained materials showed that variable photocatalyst coverage of the support surface can successfully be achieved but the photocatalytic activity towards NO removal was found to be affected by the preparation method and the nitrate selectivity is adversely affected by Ti-O-Si bonding.

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The focus of the present work is to establish means to generate and quantify levels of Ti-O-Si linkages and to correlate these with the photocatalytic properties of the supported TiO2.

界面化学键合在TiO中的作用<sub&gt; 2</sub&gt; -SiO<sub&gt; 2</sub&gt;复合材料对其光催化NOx消除性能的影响

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical ...

Detection and Quantification of Plasmodium falciparum in Aqueous Red Blood Cells by Attenuated Total Reflection Infrared Spectroscopy and Multivariate Data Analysis

We demonstrate a method of quantification and detection of parasites in aqueous red blood cells (RBCs) by using a simple benchtop Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR) spectrometer in conjunction with Multivariate Data Analysis (MVDA). 3D7 P. falciparum were cultured to 10% parasitemia ring stage parasites and used to spike fresh donor isolated RBCs to create a dilution series between 0&#8211;1%. 10 &#181;L of each sample were placed onto the center of the ATR diamond window to acquire the spectrum. The sample data was treated to improve the signal to noise ratio and to remove the contribution of water, and then the second derivative was applied to resolve spectral features. The data were then analyzed using two types of MVDA: first Principal Component Analysis (PCA) to determine any outliers and then Partial Least Squares Regression (PLS-R) to build the quantification model.

Detection and Quantification of Plasmodium falciparum in Aqueous Red Blood Cells by Attenuated Total Reflection Infrared Spectroscopy and Multivariate Data Analysis

Here, we present a protocol for the detection and quantification of Plasmodium falciparum in infected aqueous red blood cells using an attenuated total reflection infrared spectrometer and multivariate data analysis.

衰减全反射红外光谱和多变量数据分析检测和定量水红血球中恶性疟原虫

We demonstrate a method of quantification and detection of parasites in aqueous red blood cells (RBCs) by using a simple benchtop Attenuated Total ...

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the methodology for non-substituted pyridines in 1957 in a 12 h process, but no X-ray suitable crystals were obtained. The substituted ring used in the methodology presented here clearly influenced the addition of water molecules into the asymmetric unit, which confers a different nucleophilic strength in 1. The X-ray suitable crystal compound 1 was possible due to the stabilization of the negative charge in the oxygen by the presence of two water molecules where the hydrogen atoms donate positive charge into the ring; such water molecules serve well to construct a supramolecular interaction. The hydrated molecules may be possible for the alkaline system that is reached by adjusting the pH to 10. Importantly, the double methyl substituted ring and a reaction time of 5 h, makes it a more versatile method and with wider chemical applications for future ring insertions.

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

Herein, we report the synthesis and crystallization of 3,5-lutidine N-oxide dehydrate by a simple protocol that differs from the classical synthesis of pyridine N-oxide. This protocol utilizes different starting material and involves less reaction time to yield a new solvated supramolecular structure, which crystallizes under slow evaporation.

35-吡啶N-氧化物脱水的合成、结晶和光谱表征

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the ...

Preparation of Functional Silica Using a Bioinspired Method

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally purify the same by acid elution. By combining sodium silicate with a polyfunctional bioinspired additive, silica is rapidly formed at ambient conditions upon neutralization. 
The effect of neutralization rate and biomolecule addition point on silica yield are investigated, and biomolecule immobilization efficiency is reported for varying addition point. In contrast to other porous silica synthesis methods, it is shown that the mild conditions required for bioinspired silica synthesis are fully compatible with the encapsulation of delicate biomolecules. Additionally, mild conditions are used across all synthesis and modification steps, making bioinspired silica a promising target for the scale-up and commercialization as both a bare material and active support medium.
The synthesis is shown to be highly sensitive to conditions, i.e., the neutralization rate and final synthesis pH, however tight control over these parameters is demonstrated through the use of auto titration methods, leading to high reproducibility in reaction progression pathway and yield. 
Therefore, bioinspired silica is an excellent active material support choice, showing versatility towards many current applications, not limited to those demonstrated here, and potency in future applications.

Here, we present a protocol to synthesize bioinspired silica materials and immobilize enzymes therein. Silica is synthesized by combining sodium silicate and an amine &#39;additive&#39;, which neutralize at a controlled rate. Material properties and function can be altered either by in situ enzyme immobilization or post-synthetic acid elution of encapsulated additives.

用 Bioinspired 法制备功能性二氧化硅

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally ...

Inkjet Printing All Inorganic Halide Perovskite Inks for Photovoltaic Applications

A method for synthesizing photoactive inorganic&#160;perovskite quantum dot inks and an inkjet printer deposition method, using the synthesized inks, are demonstrated. The ink synthesis is based on a simple wet chemical reaction and the inkjet printing protocol is a facile step by step method. The inkjet printed thin films have been characterized by X-ray diffraction, optical absorption spectroscopy, photoluminescent spectroscopy, and electronic transport measurements. X-ray diffraction of the printed quantum dot films indicates a crystal structure consistent with an orthorhombic room temperature phase with (001) orientation. In conjunction with other characterization methods, the X-ray diffraction&#160;measurements show high quality films can be obtained through the inkjet printing method.

A protocol for synthesizing inorganic-lead-halide hybrid perovskite quantum dot inks for inkjet printing and the protocol for preparing and printing the quantum dot inks in an inkjet printer with post characterization techniques are presented.

用于光伏应用的喷墨打印所有无机舱齐德 perovskite 油墨

A method for synthesizing photoactive inorganic&#160;perovskite quantum dot inks and an inkjet printer deposition method, using the synthesized inks, are ...