Name: thermal scanning conductometry (tsc) as a general method for studying and controlling the phase behavior of conductive physical gels
Uploaded: 2018-01-23T13:30:00
Description: Watch this Scientific Journal Video about Thermal Scanning Conductometry TSC as a General Method for Studying and Controlling the Phase Behavior of Conductive Physical Gels at JoVE.com

这项工作的财政支助由国家科学中心提供, 作为赠款 No。DEC-2013/11/D/ST3/02694

1. TSC 测量试验场的制备
<ol><li>为了测量 TSC 方法的全部特性, 使用具有四电极电池的商用电导 (或者两个电极电池可以用于低电导率) 和温度传感器。将其连接至 PC, 并记录样品的导电性和温度 (4%% 甲基-46-o--基)-α-d-喃在基溴-TEABr 中的 1 M 摩尔浓度-Glyc 用于研究案例, 请参阅3款用于离子凝胶样品的制备) 以及计算机时间。</li>
	<li>对于自动读数, 使用制造商提供的软件与电导, 并设置测量模式连续与?...

<ol>
	<li>Bielejewski, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+approach+in+determination+of+ionic+conductivity+and+phase+transition+temperatures+in+gel+electrolytes+based+on+Low+Molecular+Weight+Gelators.">Novel approach in determination of ionic conductivity and phase transition temperatures in gel electrolytes based on Low Molecular Weight Gelators.</a> Electochim. Acta. 174, 1141-1148 (2015).</li><li>Bielejewski, M., &#321;api&#324;ski, A., Luboradzki, R., Tritt-Goc, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+solvent+on+the+thermal+stability+and+organization+of+self-assembling+fibrillar+networks+in+methyl-4,6-O-(p-nitrobenzylidene)-&#945;-D-glucopyranoside+gels.">Influence of solvent on the thermal stability and organization of self-assembling fibrillar networks in methyl-4,6-O-(p-nitrobenzylidene)-&#945;-D-glucopyranoside gels.</a> Tetrahedron. 67, 7222-7230 (2011).</li><li>Atsbeha, T., 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=Photophysical+characterization+of+low-molecular+weight+organogels+for+energy+transfer+and+light+harvesting.">Photophysical characterization of low-molecular weight organogels for energy transfer and light harvesting.</a> J. Mol. Struct. 993, 459-463 (2011).</li><li>Gronwald, O., Snip, E., Shinkai, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gelator+for+organic+liquids+based+on+self-assembly:+a+new+facet+of+supramolecular+and+combinatorial+chemistry.">Gelator for organic liquids based on self-assembly: a new facet of supramolecular and combinatorial chemistry.</a> Curr. Opinion in Coll. Interface Sci. 7, 148-156 (2002).</li><li>Vintiloiu, A., Leroux, 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=Organogels+and+their+use+in+drug+delivery-a+review.">Organogels and their use in drug delivery-a review.</a> Control. Rel. 125, 179-192 (2008).</li><li>Wang, Z., Fujisawa, S., Suzuki, M., Hanabusa, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Low+Molecular+Weight+Gelators+Bearing+Electroactive+Groups+as+Cathode+Materials+for+Rechargeable+Batteries.">Low Molecular Weight Gelators Bearing Electroactive Groups as Cathode Materials for Rechargeable Batteries.</a> Macromol. Symp. 364, 38-46 (2016).</li><li>Sharma, N., 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=Physical+gels+of+[BMIM][BF4]+by+N-tert-butylacrylamide/ethylene+oxide+based+triblock+copolymer+self-assembly:+Synthesis,+thermomechanical,+and+conducting+properties.">Physical gels of [BMIM][BF4] by N-tert-butylacrylamide/ethylene oxide based triblock copolymer self-assembly: Synthesis, thermomechanical, and conducting properties.</a> J. Appl. Polym. Sci. 128, 3982-3992 (2013).</li><li>Tao, L., 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=Stable+quasi-solid-state+dye-sensitized+solar+cell+using+a+diamide+derivative+as+low+molecular+mass+organogelator.">Stable quasi-solid-state dye-sensitized solar cell using a diamide derivative as low molecular mass organogelator.</a> J. Power Sources. 262, 444-450 (2014).</li><li>Kataoka, T., Ishioka, Y., Mizuhata, M., Minami, H., Maruyama, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Highly+Conductive+Ionic-Liquid+Gels+Prepared+with+Orthogonal+Double+Networks+of+a+Low-Molecular-Weight+Gelator+and+Cross-Linked+Polymer.">Highly Conductive Ionic-Liquid Gels Prepared with Orthogonal Double Networks of a Low-Molecular-Weight Gelator and Cross-Linked Polymer.</a> ACS Appl. Mater. Interfaces. 7, 23346-23352 (2015).</li><li>Bielejewski, M., Nowicka, K., Bielejewska, N., Tritt-Goc, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+Conductivity+and+Thermal+Properties+of+a+Supramolecular+Ionogel+Made+from+a+Sugar-Based+Low+MolecularWeight+Gelator+and+a+Quaternary+Ammonium+Salt+Electrolyte+Solution.">Ionic Conductivity and Thermal Properties of a Supramolecular Ionogel Made from a Sugar-Based Low MolecularWeight Gelator and a Quaternary Ammonium Salt Electrolyte Solution.</a> J. Electrochem. Soc. 163, G187-G195 (2016).</li><li>Gronwald, O., Shinkai, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bifunctional'+sugar-integrated+gelators+for+organic+solvents+and+water-on+the+role+of+nitro-substituents+in+1-O-methyl-4,6-O-(nitrobenzylidene)-monosaccharides+for+the+improvement+of+gelation+ability.">Bifunctional' sugar-integrated gelators for organic solvents and water-on the role of nitro-substituents in 1-O-methyl-4,6-O-(nitrobenzylidene)-monosaccharides for the improvement of gelation ability.</a> J. Chem. Soc., Perkin Trans. 2, 1933-1937 (2001).</li><li>Bielejewski, M., Ghorbani, M., Zolfigol, M., Tritt-Goc, J., Noura, S., Narimani, M., Oftadeh, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermally+reversible+solidification+of+novel+ionic+liquid+[im]HSO4+by+self-nucleated+rapid+crystallization:+investigations+of+ionic+conductivity,+thermal+properties,+and+catalytic+activity.">Thermally reversible solidification of novel ionic liquid [im]HSO4 by self-nucleated rapid crystallization: investigations of ionic conductivity, thermal properties, and catalytic activity.</a> RSC Adv. 6, 108896-108907 (2016).</li></ol>

热扫描电导是一种新的实验方法, 它被证明是一种有效和有效的方法来调查动态变化的系统, 如 ionogels 的基础上低分子量胶, 电解质, 或离子液体。然而, 它的适用性不仅限于 ionogels。TSC 方法可以很容易地与其他类型的导电软物质系统, 如水凝胶, 乳液, 药膏, 或任何其他电荷含有的载体, 电导传感器可以插入。该方法的局限性在于它依赖于电导率传感器本身, 以及它可以使用的样本类型, 但是该协议?...

热可逆 Ionogels 物理胶凝是一个过程, 允许结构的自组装胶分子存在的溶剂分子。由于这种现象的相互作用的非共价键性质 (如氢键、范德华相互作用、色散力、静电力、ππ叠加、等), 这些系统是热可逆的。这种热可逆性, 连同胶的极低浓度和可以被创造的系统的各种各样, 是物理凝胶的一些主要好处在化工部分。由于物理凝胶状态的独特性质, ionogels 的特点是可取的特点, 如易于回收, 长周期寿命, 增强的物理性能 (例如离子电导率), 易于生产, 并降低生产成本。考虑到上述物理凝胶的优点 (已经有广泛的不同应用范围1,2,3,4), 这些都被认为是用来替代电解质固化和获得 ionogels5,6,7,8。然而, 经典的电导是不敏感和准确的, 足以跟踪这样的动态变化的系统。因此, 它无法检测凝胶基质中离子的相变和增强动力学9。这种不敏感的原因是温度稳定所需要的时间, 在此期间, 在开始测量之前, 样品的动态变化正在进行。此外, 测量的温度的数量是有限的顺序, 而不是显着延长实验时间。因此, 为了充分准确地刻画 ionogels, 需要一种新的方法, 它可以跟踪性能的动态变化作为温度的函数, 并能实时记录数据。进行凝胶过程的方式决定了所创建的 ionogel 的性质。在冷却阶段定义了分子间非共价键相互作用;通过改变凝胶温度和冷却速率, 人们可以强烈地影响这些相互作用。因此, 当凝胶发生时, 在冷却过程中测量系统是极其重要的。经典的方法, 这是不可能的, 因为温度稳定时间的测量, 和快速冷却率所需的成功凝胶。然而, 用热扫描电导方法这项任务是非常简单的, 提供准确和可重现的结果, 并允许研究不同的热变化动力学的影响应用于样品的样品属性10. 因此, 具有目标属性的 ionogels 可以同时进行研究和制造。
热扫描电导 (TSC) 热扫描电导应该提供一个可重现的, 准确的, 快速的反应实验方法的动态变化和热可逆系统的电导率测量, 如 ionogels 基于低分子量胶.然而, 它也可以用于电解质, 离子液体, 和任何其他导电样品, 可以放在测量细胞, 并具有电导率的传感器的测量范围。此外, 该方法除研究应用外, 还成功地用于制造具有显微组织、光学外观或热稳定性等目标性质的 ionogels, 并能准确、简便地实现相变温度。利用 TSC 法进行热处理的动力学和历史, 对物理凝胶系统的一些基本特性进行了全面的控制。此外, 该室还配备了一个摄像机, 以检查样品的状态和记录的变化, 特别是在凝胶和溶解过程中的样品。TSC 方法的另一个优点是它的简单性, 因为该系统可以建立在一个标准的电导, 可编程温度控制器, 气体氮气线的加热/冷却介质, 冰箱, 测量室, 和 PC,可以在大多数实验室中找到。
TSC 实验场 热扫描电导实验装置可以建立在几乎每个实验室, 成本相对较低。作为回报, 你得到一个准确的, 可重现的, 快速的方法来测量液体和半固态导电样品在不同的外部条件。在我们的实验室中建立的 TSC 实验装置的详细方案在图 1中给出。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56607/56607fig1v2.jpg"> 图 1: 测量站点的框图.热扫描电导方法的工作实验装置组成。<a href="//cloudflare.jove.com/files/ftp_upload/56607/56607fig1v2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
对于温度的变化, 采用自制的温度控制器, 可采用可编程的温度控制器, 可以用定义的变化率线性改变温度。对于热隔离, 已经建立了一个特殊的腔室。使用隔离室的目的是尽量减少样品中的温度水平梯度, 并保证快速冷却速率。该室由一个直径为40毫米的玻璃圆筒和300毫米的长度组成。在底部, 气体氮气进口加热器位于, 入口的末端装备了压均匀地传播热或冷气体。这也是温度传感器 PT100 的地方在可变温度控制器 (职训局) 位于。样品的温度由位于电导传感器中的温度传感器独立记录。此外, 该室还配备了一个摄像机, 以检查样品的状态和记录的变化, 特别是在凝胶和溶解过程中的样品。采用 250 L 高压贮罐中液氮蒸发所获得的气态氮作为加热和冷却介质。在氮气线的工作压力设置为6条, 并减少到2酒吧在测量现场。这样的设置允许在4和28升/分钟之间的流量取得没有任何干扰, 这使得冷却率为10° c/分钟。为了降低氮气的初始温度, 采用了外部制冷机, 降低了温度为10° c。这使得从室温开始的温度变化具有良好的线性度。在快速冷却期间, 氮气的温度降低到-15 ° c, 以协助高冷却率。由于低温, 必须使用气态氮, 而不是干燥的空气, 以避免结冰的冰箱。
样品入了 9 毫米内径和长度 58 毫米的小瓶 , 由聚丙烯制成 , 并且装备了螺丝盖帽 , 有橡胶圆环为严密的关闭。小瓶可以使用由120° c。(请参见图 2)。
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56607/56607fig2.jpg"> 图 2: 聚丙烯小瓶的图片及其在电导率传感器上的安装.(1) 聚丙烯小瓶, (2) 带橡胶圈的螺丝盖, 2a-安装在导电性传感器上的螺钉盖, (3) 装有电导传感器的小瓶, 用聚四氟乙烯胶带固定的螺钉盖。<a href="//cloudflare.jove.com/files/ftp_upload/56607/56607fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

<table border="0" cellpadding="0" cellspacing="0" width="698">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">SevenCompact S230 conductometer</td>
			<td style="width:140px;">Mettler-Toledo</td>
			<td style="width:119px;"></td>
			<td style="width:223px;">equiped with InLab 710 sensor</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">home-build VTC</td>
			<td style="width:140px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:216px;">LabX PH 3.2 software</td>
			<td style="width:140px;">Mettler-Toledo</td>
			<td style="width:119px;"></td>
			<td>software used for data aqusition</td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:216px;">tetraethylammonium bromide</td>
			<td style="width:140px;">Sigma-Aldrich</td>
			<td style="width:119px;">140023</td>
			<td></td>
		</tr>
		<tr height="30">
			<td height="30" style="height:30px;width:216px;">glycerol</td>
			<td style="width:140px;">Sigma-Aldrich</td>
			<td style="width:119px;">G5516</td>
			<td></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:216px;">methyl-4,6-O-(p-nitrobenzylidene)-a-D-glucopyranose</td>
			<td style="width:140px;"></td>
			<td style="width:119px;"></td>
			<td style="width:223px;">synthezied according to Gronwald, O., Shinkai, S., J. chem. Soc., Perkin Trans. 2 1933-1937 (2001).</td>
		</tr>
		<tr height="201">
			<td height="201" style="height:201px;width:216px;">[im]HSO4</td>
			<td style="width:140px;"></td>
			<td style="width:119px;"></td>
			<td style="width:223px;">synthezeid by group of prof. Mohammad Ali Zolfigol, Faculty of Chemistry 
			Bu-Ali Sina University 
			Hamedan, I.R.Iran&#160; according to Bielejewski, M., Ghorbani, M., Zolfigol, M., Tritt-Goc, J., Noura, S., Narimani, M., Oftadeh, M. RSC Adv. 6, 108896-108907 (2016).</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">polypropylene vial</td>
			<td style="width:140px;">Paradox Company, Cracow, Poland</td>
			<td style="width:119px;">PTC 088</td>
			<td>www.insectnet.eu</td>
		</tr>
	</tbody>
</table>

thermal scanning conductometry (tsc) as a general method for studying and controlling the phase behavior of conductive physical gels

热扫描电导协议是研究基于低分子量胶的离子凝胶的一种新方法。该方法的目的是跟踪 ionogels 的动态变化状态, 并提供更多的信息和细节的微妙变化的导电性能随着温度的增减。此外, 该方法还允许在恒定温度下进行长期 (即天、周) 测量, 以调查系统的稳定性和耐久性以及老化效应。TSC 方法的主要好处在古典电导是能力执行测量在胶凝过程期间, 是不可能的以古典方法由于温度稳定, 通常需要很长时间在个人测量。获得物理凝胶相是一个众所周知的事实, 冷却阶段必须是快速的;此外, 根据冷却速度, 可以实现不同的显微结构。TSC 方法可以进行任何冷却/加热速率, 可由外部温度系统保证。在我们的情况下, 我们可以实现线性温度变化率在0.1 和大约10° c/分钟之间。热扫描电导设计为循环工作, 在加热和冷却阶段之间不断变化。这种方法可以研究热可逆凝胶溶胶相变的重现性。此外, 它允许在同一样本上的不同实验协议的性能, 可以刷新到初始状态 (如果有必要) 不从测量单元中删除。因此, 测量可以更快、更有效地执行, 并且具有更高的重现性和精确性。此外, TSC 方法也可以作为一种工具, 制造 ionogels 的目标性质, 如微观结构, 即时表征导电性能。

有机离子凝胶构成了一种新型的功能材料, 可以成为高分子凝胶电解质的替代溶液。然而, 为了达到这个目的, 这些凝胶必须被深入研究和理解。凝胶过程的热可逆特性, 以及温度和相位发生的动态变化特性, 需要一种新的实验方法, 使数据的记录和温度的细微变化的检测更改.热扫描电导是唯一的方法, 允许记录的电导率和温度的样品在加热冷却循环, 和线性变化的温度。TSC ?...

Watch this Scientific Journal Video about Thermal Scanning Conductometry TSC as a General Method for Studying and Controlling the Phase Behavior of Conductive Physical Gels at JoVE.com

Thermal Scanning Conductometry TSC as a General Method for Studying and Controlling the Phase Behavior of Conductive Physical Gels

冷却过程的动力学定义了基于低分子量胶的离子凝胶的性质。这份手稿描述了热扫描电导 (TSC) 的使用, 它得到完全控制的凝胶过程, 连同原位测量样品的温度和电导率。

热扫描电导 (TSC) 作为研究和控制导电物理凝胶相行为的一般方法

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Thermal Scanning Conductometry (TSC) as a General Method for Studying and Controlling the Phase Behavior of Conductive Physical Gels

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A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants

对水样的自动固相萃取小污染物的免疫学分析的简单方法

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and ...

LC-MS Analysis of Human Platelets as a Platform for Studying Mitochondrial Metabolism

Perturbed mitochondrial metabolism has received renewed interest as playing a causative role in a range of diseases. Probing alterations to metabolic ...

Protocol for Measuring the Thermal Properties of a Supercooled Synthetic Sand-water-gas-methane Hydrate Sample

协议测量过冷的合成砂水 - 气 - 甲烷水合物样品的热性能

Methane hydrates (MHs) are present in large amounts in the ocean floor and permafrost regions. Methane and hydrogen hydrates are being studied as future ...

A Bending Test for Determining the Atterberg Plastic Limit in Soils

弯曲试验在土壤确定阿太堡限塑

The thread rolling test is the most commonly used method to determine the plastic limit (PL) in soils. It has been widely criticized, because a ...

Metal Corrosion and the Efficiency of Corrosion Inhibitors in Less Conductive Media

金属腐蚀与腐蚀抑制剂在低导电介质中的效率

Material corrosion can be a limiting factor for different materials in many applications. Thus, it is necessary to better understand corrosion processes, ...

A Loop-mediated Isothermal Amplification (LAMP) Assay for Rapid Identification of Bemisia tabaci

A Loop-mediated Isothermal Amplification LAMP Assay for Rapid Identification of Bemisia tabaci

循环介导等温扩增 (灯管) 法快速识别烟粉虱

The whitefly Bemisia tabaci (Gennadius) is an invasive pest of considerable importance, affecting the production of vegetable and ornamental crops in many ...