Financial support for this work was provided by the National Center for Science as grant No. DEC-2013/11/D/ST3/02694.

1. Preparation of the Experimental Site for TSC Measurement
<ol>
	<li>To measure the full characteristics of the TSC method, use the commercially available conductometer equipped with four electrode cells (alternatively, two electrode cells can be used for low conductivities) and a temperature sensor. Connect it to the PC and record the conductivity and temperature of the sample (4% wt% of methyl-4,6-O-(p-nitrobenzylidene)-&#945;-D-glucopyranoside in 1 M molar concentration of tetraethylammonium bromide - TEABr in glycerol - Glyc used in studied case, see paragraph 3 for ionic gel sample preparation) along with computer time.</li>
	<li>For automatic readouts, use the software supplied by the manufacturer along with the conductometer, and set the measuring mode to continuous with interval readings every 1 s.</li>
	<li>Prepare the nitrogen line (fill the high-pressure nitrogen tank with liquid nitrogen and start to evaporate it to get gaseous nitrogen in the nitrogen line), and set the pressure to 2 bars and required flow, then decrease the initial temperature of the nitrogen gas with the aid of a refrigerator.</li>
	<li>Tightly mount the screw cap of the vial on the conductive sensor, and secure it with a piece of teflon tape (crucial with volatile samples) (see Figure 2).</li>
</ol>
2. Preparation of Electrolyte Solution
<ol>
	<li>Prepare the electrolytes by mixing an appropriate amount of glycerol, used as a solvent, and tetraethylammonium bromide (TEABr) (use scale to weigh the required amount of compounds accordingly for the concentration needed for investigation), used as a solute, in a glass vial tightly closed and heated at 100 &#176;C for 15 min.</li>
	<li>Next, stir the mixture for 1 min and heat it again at 100 &#176;C for 5 min to ensure that all the solute is dissolved and the mixture is homogeneous.</li>
	<li>Use these prepared electrolyte solutions for measurements, and afterwards for preparation of ionogels.</li>
</ol>
3. Preparation of Low Molecular Weight Ionic Gels
<ol>
	<li>Prepare the ionogels from the electrolyte solutions (see section 2) by adding 178.6 mg of the low molecular weight gelator to 4 mL of 1 M TEABr/Glyc electrolyte solution to obtain 4% wt% of ionic gel sample. 
	NOTE: The chemical synthesis of the used gelator was described elsewhere11.</li>
	<li>To dissolve the gelator, add it to the glass vial with the electrolyte solution and heat it at 130 &#176;C for 20 min with additional stirring to assist dissolution.</li>
	<li>After completely dissolving the gelator, heat the mixture for an additional 5 min to ensure the sample is homogenous.</li>
	<li>Next, quickly cool down the sample in a dry cooling block at 10 &#176;C to ensure physical gelation. After the procedure, a homogeneous, transparent, or opaque gel phase should be obtained (Figure 3). 
	NOTE: After the first gelation has been performed, the sample becomes liquid when turning to sol phase at high temperatures, but after returning to room temperature it turns to the gel phase again. The temperature needed for the gel-sol phase transition is lower than the temperature needed for dissolution of the crystalline gelator. By changing the kinetics of the cooling stage, one can influence the physical properties of the obtained ionogel, like microstructure, optical appearance, or the gel-sol phase transition temperature (Tgs).</li>
</ol>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/56607/56607fig3.jpg" /> 
Figure 3: The physical appearance of the investigated sample. The 1M TEABr/Glyc electrolyte (a), 4% ionogel with 1M TEABr/Glyc electrolyte in transparent phase (b), 4% ionogel with 1M TEABr/Glyc electrolyte in opaque phase (c). <a href="//cloudfront.jove.com/files/ftp_upload/56607/56607fig3large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
4. In Situ Thermal Scanning Conductometry of Ionogels
<ol>
	<li>To prepare the sample for TSC measurement, heat the ionogel above the Tgs temperature, 94.85 &#176;C in the studied case. Transfer it to the precooled polypropylene vial after it turns to sol phase. Due to the fast cooling down of the sol, the gel phase is created.</li>
	<li>Insert the conductivity sensor (with the screw cap of the vial on it) into the vial by pushing it into the gel, tighten the screw cap, and secure it with Teflon tape.</li>
	<li>Perform the TSC measurement and record conductivity, temperature, and time to prepare conductivity vs temperature, temperature vs time, and conductivity vs time dependencies. Repeat the measurement in the investigated temperature range (9.85 - 99.85 &#176;C) in heating-cooling cycles (at least 2 times). 
	NOTE: Remember the 1st cycle is used to eliminate all discrepancies of the sample caused by the preparation procedure.</li>
	<li>Perform the measurements with different cooling rates (7 &#176;C/min, 4 &#176;C/min, and 1 &#176;C/min in studied case) to explore how it influences the conductive and thermal properties of investigated ionogels. 
	NOTE: To demonstrate how the TSC method can be used as a tool to obtain ionogels with targeted properties, a series of experiments with non-aqueous ionogel based on gelator 1, glycerol, and TEABr was performed and presented in this manuscript.</li>
</ol>
5. Example of TSC Measurement
<ol>
	<li>Insert the investigated ionogel into the vial, and push in the conductivity sensor.</li>
	<li>Perform the 1st heating-cooling cycle to improve the electrode contact, and remove all imperfections of the ionogel microstructure resulting from placing the sample in the vial and seen as scratches, cracks, and air bubbles included in the gel.</li>
	<li>Measure the conductivity and temperature along with time during the 2nd and 3rd heating-cooling cycle to investigate the performance of the ionogel, and the reproducibility of the system. Set the heating rate to 2 &#176;C/min and cooling rate to 7 &#176;C/min, and gelation temperature to 10 &#176;C. As a result, obtain a transparent gel phase.</li>
	<li>Perform the 4th and 5th heating-cooling cycle, with the heating and cooling rates equal to 2 &#176;C/min, and the gelation temperature equal to 10 &#176;C. As a result, obtain a mixture of the transparent and opaque gel phases.</li>
	<li>Perform the 6th and 7th heating-cooling cycle with heating and cooling rates equal to 2 &#176;C/min, and a gelation temperature equal to 60 &#176;C. As a result, obtain an opaque, white gel phase.</li>
	<li>Perform the analysis of the 1st derivatives for recorded data to see differences between samples.</li>
	<li>Keep the sample for 20 min at each of the gelation temperatures to ensure that the gelation process is completed.</li>
</ol>

<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>

The author has nothing to disclose

The thermal scanning conductometry is a new experimental method which has proven to be an efficient and effective way of investigating dynamically changing systems, like ionogels based on low molecular weight gelators, electrolytes, or ionic liquids. However, its applicability is not restricted only to ionogels. The TSC method can be easily used with other types of conducting soft matter systems like hydrogels, emulsions, creams, or any other charge containing carriers into which the conductivity sensor can be inserted. ...

Thermally Reversible Ionogels 
Physical gelation is a process which allows the construction of structures of self-assembled gelator molecules in presence of the solvent molecules. Due to non-covalent nature of the interactions responsible for this phenomenon (e.g. hydrogen bonding, van der Waals interactions, dispersion forces, electrostatic forces, &#960;-&#960; stacking, etc.), these systems are thermally reversible. This thermal reversibility, together with the very low concentration of the gelator and the wide variety of the systems that can be created, are some of the main advantages of physical gels over chemical ones. Thanks to the unique properties of the physical gel state, the ionogels are characterized with desirable features like easy recycling, long cycle life, enhanced physical properties (e.g. ionic conductivity), ease of production, and lowering of the production costs. Taking into the account the above advantages of physical gels (which already have a wide range of different applications1,2,3,4), these were thought to be used as an alternative way for electrolyte solidification and obtaining of ionogels5,6,7,8. However, the classical conductometry was not sensitive and accurate enough to follow such dynamically changing systems. Therefore,it could not detect the phase transitions and enhanced dynamics of ions in the gel matrix9. The reason for this insensitivity was the time needed for the temperature stabilization, during which dynamic changes of the sample properties were underway before the measurement was started. Furthermore, the number of measured temperatures was limited in order, not to significantly extend the experimental time. Therefore, to fully and accurately characterize the ionogels, a new method was needed, which would be able to follow the dynamic changes of properties as a function of temperature, and record data continuously in real time. The way the gelation process is conducted determines the properties of the created ionogel. The intermolecular non-covalent interactions are defined during the cooling stage; by changing the gelation temperature and cooling rates, one can strongly influence those interactions. Therefore, it was extremely important to measure the system during cooling when the gelation takes place. With the classical approach, this was impossible due to temperature stabilization time for the measurement, and the fast cooling rates required for successful gelation. However, with the thermal scanning conductometry method this task is very simple, delivers accurate and reproducible results, and allows the investigation of the influence of different kinetics of thermal changes applied to the sample on sample properties10. As a result, the ionogels with targeted properties can be studied and manufactured at the same time.
Thermal Scanning Conductometry (TSC) 
The thermal scanning conductometry is supposed to deliver a reproducible, accurate, and fast responding experimental method for the conductivity measurement of dynamically changing and thermally reversible systems, like ionogels based on low molecular weight gelators. However, it can be also used with electrolytes, ionic liquids, and any other conducting sample that can be placed in the measuring cell and has conductivity in the measuring range of the sensor. Additionally, besides the research application, the method was successfully used to manufacture ionogels with targeted properties like microstructure, optical appearance or thermal stability, and phase transition temperature in an accurate and easy way. Depending on the kinetics and history of thermal treating with use of the TSC method, we gain full control over some basic properties of physical gel systems. Additionally the chamber have been equipped in a video camera to inspect the sample state and record the changes of the sample especially during gelation and dissolution processes. An additional advantage of the TSC method is its simplicity, as the system can be built from a standard conductometer, a programmable temperature controller, the gaseous nitrogen line for the heating/cooling medium, the refrigerator, measuring chamber, and a PC, which can be found in most laboratories.
The TSC Experimental Site 
The thermal scanning conductometry experimental setup can be built in almost every laboratory with relatively low costs. In return, one obtains an accurate, reproducible, and fast method for measuring liquid and semisolid conductive samples at different external conditions. A detailed scheme of the TSC experimental setup built in our laboratory is given in Figure 1.
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56607/56607fig1v2.jpg" /> 
Figure 1: Block diagram of the measurement site. The components consisting on working experimental setup for thermal scanning conductometry method. <a href="//cloudflare.jove.com/files/ftp_upload/56607/56607fig1v2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
For the temperature change, a homemade temperature controller was used, but any kind of programmable temperature controller, which can change the temperature linearly with a defined change rate, can be used. For thermal isolation, a special chamber has been built. The purpose of using an isolation chamber is to minimize temperature horizontal gradients in the sample, and to assure fast cooling rates. The chamber consists of a glass cylinder with a 40-mm inner diameter and 300 mm length. At the bottom side, where the heater with gaseous nitrogen inlets are located, the end of the inlet is equipped with a diffusor to evenly spread the hot or cold gas. This is also the place where the temperature sensor PT100 of the variable temperature controller (VTC) is located. The temperature of the sample is recorded independently by the temperature sensor located in the conductivity sensor. Additionally, the chamber have been equipped in a video camera to inspect the sample state and record the changes of the sample especially during gelation and dissolution processes. The gaseous nitrogen obtained from evaporation of liquid nitrogen in the 250 L high pressure tank is used as a heating and cooling medium. The working pressure in the nitrogen line is set to 6 bars, and reduced to 2 bars at the measuring site. Such settings allow the obtainment of flow rates between 4 and 28 L/min without any disturbances, which allows a cooling rate of 10 &#176;C/min. To lower the initial temperature of the nitrogen gas, the external refrigerator has been used, and the decreased temperature was 10 &#176;C. This allows the obtainment of good linearity of the temperature change, starting from room temperature. During fast cooling, the temperature of the nitrogen gas is decreased to -15 &#176;C to assist high cooling rates. It is necessary to use gaseous nitrogen, and not even dry air, to avoid icing the refrigerator because of low temperatures.
The samples were inserted into a vial of 9 mm inner diameter and length of 58 mm, made of polypropylene, and equipped with a screw cap, which has a rubber ring for tight closing. The vials can be used up to 120 &#176;C. (see Figure 2).
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56607/56607fig2.jpg" /> 
Figure 2: The picture of a polypropylene vial and its mounting on the conductivity sensor. (1) the polypropylene vial, (2) the screw cap with rubber ring, 2a - the screw cap mounted on the conductivity sensor, (3) the vial with mounted conductivity sensor, the screw cap secured with Teflon tape. <a href="//cloudflare.jove.com/files/ftp_upload/56607/56607fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</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

The thermal scanning conductometry protocol is a new approach in studying ionic gels based on low molecular weight gelators. The method is designed to follow the dynamically changing state of the ionogels, and to deliver more information and details about the subtle change of conductive properties with an increase or decrease in the temperature. Moreover, the method allows the performance of long term (i.e. days, weeks) measurements at a constant temperature to investigate the stability and durability of the system and the aging effects. The main advantage of the TSC method over classical conductometry is the ability to perform measurements during the gelation process, which was impossible with the classical method due to temperature stabilization, which usually takes a long time before the individual measurement. It is a well-known fact that to obtain the physical gel phase, the cooling stage must be fast; moreover, depending on the cooling rate, different microstructures can be achieved. The TSC method can be performed with any cooling/heating rate that can be assured by the external temperature system. In our case, we can achieve linear temperature change rates between 0.1 and approximately 10 &#176;C/min. The thermal scanning conductometry is designed to work in cycles, continuously changing between heating and cooling stages. Such an approach allows study of the reproducibility of the thermally reversible gel-sol phase transition. Moreover, it allows the performance of different experimental protocols on the same sample, which can be refreshed to initial state (if necessary) without removal from the measuring cell. Therefore, the measurements can be performed faster, in a more efficient way, and with much higher reproducibility and accuracy. Additionally, the TSC method can be also used as a tool to manufacture the ionogels with targeted properties, like microstructure, with an instant characterization of conductive properties.

The organic ionic gels constitute a new class of functional materials which can become an alternative solution for polymer gel electrolytes. However, to achieve this aim, these gels have to be deeply investigated and understood. The thermally reversible character of the gelation process, and the dynamically changing properties of temperature and phase occurrence, required a new experimental method which will allow the recording of data and detection of subtle changes in temperature change...

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

The kinetics of the cooling process defines the properties of ionic gels based on low molecular weight gelators. This manuscript describes the usage of thermal scanning conductometry (TSC), which obtains full control over the gelation process, along with in situ measurements of the samples' temperature and conductivity.

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

The thermal scanning conductometry protocol is a new approach in studying ionic gels based on low molecular weight gelators. The method is designed to ...

thermal-scanning-conductometry-tsc-as-general-method-for-studying

Research

JoVE Journal

Environment

7.6K Views.  Institute of Molecular Physics Polish Academy of Sciences. The kinetics of the cooling process defines the properties of ionic gels based on low molecular weight gelators. This manuscript describes the usage of thermal scanning conductometry (TSC), which obtains full control over the gelation process, along with in situ measurements of the samples' temperature and conductivity. 

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

A Noninvasive Method For In situ Determination of Mating Success in Female American Lobsters (Homarus americanus)

Despite being one of the most productive fisheries in the Northwest Atlantic, much remains unknown about the natural reproductive dynamics of American lobsters. Recent work in exploited crustacean populations (crabs and lobsters) suggests that there are circumstances where mature females are unable to achieve their full reproductive potential due to sperm limitation. To examine this possibility in different regions of the American lobster fishery, a reliable and noninvasive method was developed for sampling large numbers of female lobsters at sea. This method involves inserting a blunt-tipped needle into the female&#39;s seminal receptacle to determine the presence or absence of a sperm plug and to withdraw a sample that can be examined for the presence of sperm. A series of control studies were conducted at the dock and in the laboratory to test the reliability of this technique. These efforts entailed sampling 294 female lobsters to confirm that the presence of a sperm plug was a reliable indicator of sperm within the receptacle and thus, mating. This paper details the methodology and the results obtained from a subset of the total females sampled. Of the 230 female lobsters sampled from George&#39;s Bank and Cape Ann, MA (size range = 71-145 mm in carapace length), 90.3% were positive for sperm. Potential explanations for the absence of sperm in some females include: immaturity (lack of physiological maturity), breakdown of the sperm plug after being used to fertilize a clutch of eggs, and lack of mating activity. The surveys indicate that this technique for examining the mating success of female lobsters is a reliable proxy that can be used in the field to document reproductive activity in natural populations.

A Noninvasive Method For In situ Determination of Mating Success in Female American Lobsters Homarus americanus

Fishery-induced changes to exploited crustacean fisheries, such as the American lobster fishery, could potentially influence their reproductive dynamics, leading to a reduction in mating success. This study&#39;s goal was to develop a noninvasive method for ascertaining the mating success of female lobsters that may be physiologically or functionally mature.

Despite being one of the most productive fisheries in the Northwest Atlantic, much remains unknown about the natural reproductive dynamics of American ...

Technique for Studying Arthropod and Microbial Communities within Tree Tissues

Phloem tissues of pine are habitats for many thousands of organisms. Arthropods and microbes use phloem and cambium tissues to seek mates, lay eggs, rear young, feed, or hide from natural enemies or harsh environmental conditions outside of the tree. Organisms that persist within the phloem habitat are difficult to observe given their location under bark. We provide a technique to preserve intact phloem and prepare it for experimentation with invertebrates and microorganisms. The apparatus is called a &#8216;phloem sandwich&#8217; and allows for the introduction and observation of arthropods, microbes, and other organisms. This technique has resulted in a better understanding of the feeding behaviors, life-history traits, reproduction, development, and interactions of organisms within tree phloem. The strengths of this technique include the use of inexpensive materials, variability in sandwich size, flexibility to re-open the sandwich or introduce multiple organisms through drilled holes, and the preservation and maintenance of phloem integrity. The phloem sandwich is an excellent educational tool for scientific discovery in both K-12 science courses and university research laboratories.

We provide a technique to preserve intact tree phloem and prepare it for observation. We create an apparatus called a phloem sandwich that allows for the introduction and observation of arthropods, microbes, and other organisms that inhabit phloem tissues.

Phloem tissues of pine are habitats for many thousands of organisms.  Arthropods and microbes use phloem and cambium tissues to seek mates, lay eggs, rear ...

Physical, Chemical and Biological Characterization of Six Biochars Produced for the Remediation of Contaminated Sites

The physical and chemical properties of biochar vary based on feedstock sources and production conditions, making it possible to engineer biochars with specific functions (e.g. carbon sequestration, soil quality improvements, or contaminant sorption). In 2013, the International Biochar Initiative (IBI) made publically available their Standardized Product Definition and Product Testing Guidelines (Version 1.1) which set standards for physical and chemical characteristics for biochar. Six biochars made from three different feedstocks and at two temperatures were analyzed for characteristics related to their use as a soil amendment. The protocol describes analyses of the feedstocks and biochars and includes: cation exchange capacity (CEC), specific surface area (SSA), organic carbon (OC) and moisture percentage, pH, particle size distribution, and proximate and ultimate analysis. Also described in the protocol are the analyses of the feedstocks and biochars for contaminants including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), metals and mercury as well as nutrients (phosphorous, nitrite and nitrate and ammonium as nitrogen). The protocol also includes the biological testing procedures, earthworm avoidance and germination assays. Based on the quality assurance / quality control (QA/QC) results of blanks, duplicates, standards and reference materials, all methods were determined adequate for use with biochar and feedstock materials. All biochars and feedstocks were well within the criterion set by the IBI and there were little differences among biochars, except in the case of the biochar produced from construction waste materials. This biochar (referred to as Old biochar) was determined to have elevated levels of arsenic, chromium, copper, and lead, and failed the earthworm avoidance and germination assays. Based on these results, Old biochar would not be appropriate for use as a soil amendment for carbon sequestration, substrate quality improvements or remediation.

Biochar is a carbon-rich material used as a soil amendment with the ability to sustainably sequester carbon, improve substrate quality and sorb contaminants. This protocol describes the 17 analytical methods used for the characterization of biochar, which is required prior to large scale implementation of these amendments in the environment.

The physical and chemical properties of biochar vary based on feedstock sources and production conditions, making it possible to engineer biochars with ...

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

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17&#946;-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 &#181;l of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

A protocol for the extraction and pre-concentration of estradiol from water samples by using an automated and miniaturized system is presented.

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 pathways requires a model in which external factors can be well controlled, allowing for reproducible and meaningful results. Many studies employ transformed cellular models for these purposes; however, metabolic reprogramming that occurs in many cancer cell lines may introduce confounding variables. For this reason primary cells are desirable, though attaining adequate biomass for metabolic studies can be challenging. Here we show that human platelets can be utilized as a platform to carry out metabolic studies in combination with liquid chromatography-tandem mass spectrometry analysis. This approach is amenable to relative quantification and isotopic labeling to probe the activity of specific metabolic pathways. Availability of platelets from individual donors or from blood banks makes this model system applicable to clinical studies and feasible to scale up. Here we utilize isolated platelets to confirm previously identified compensatory metabolic shifts in response to the complex I inhibitor rotenone. More specifically, a decrease in glycolysis is accompanied by an increase in fatty acid oxidation to maintain acetyl-CoA levels. Our results show that platelets can be used as an easily accessible and medically relevant model to probe the effects of xenobiotics on cellular metabolism.

Here we show isolated human platelets can be used as an accessible ex vivo model to study metabolic adaptations in response to the complex I inhibitor rotenone. This approach employs isotopic tracing and relative quantification by liquid chromatography-mass spectrometry and can be applied to a variety of study designs.

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

Methane hydrates (MHs) are present in large amounts in the ocean floor and permafrost regions. Methane and hydrogen hydrates are being studied as future energy resources and energy storage media. To develop a method for gas production from natural MH-bearing sediments and hydrate-based technologies, it is imperative to understand the thermal properties of gas hydrates.
The thermal properties' measurements of samples comprising sand, water, methane, and MH are difficult because the melting heat of MH may affect the measurements. To solve this problem, we performed thermal properties' measurements at supercooled conditions during MH formation. The measurement protocol, calculation method of the saturation change, and tips for thermal constants' analysis of the sample using transient plane source techniques are described here.
The effect of the formation heat of MH on measurement is very small because the gas hydrate formation rate is very slow. This measurement method can be applied to the thermal properties of the gas hydrate-water-guest gas system, which contains hydrogen, CO2, and ozone hydrates, because the characteristic low formation rate of gas hydrate is not unique to MH. The key point of this method is the low rate of phase transition of the target material. Hence, this method may be applied to other materials having low phase-transition rates.

We present a protocol for measuring the thermal properties of synthetic hydrate-bearing sediment samples comprising sand, water, methane, and methane hydrate.

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

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 considerable subjective judgment from the operator that carries out the test is involved during its performance, which may affect the final result significantly. Different alternative methods have been put forward, but they cannot compete with the standard rolling test in speed, simplicity and cost.
In an earlier study by the authors, a simple method with a simple device to determine the PL was presented (the &#34;thread bending test&#34; or simply &#34;bending test&#34;); this method allowed the PL to be obtained with minimal operator interference. In the present paper a version of the original bending test is shown. The experimental basis is the same as the original bending test: soil threads which are 3 mm in diameter and 52 mm long are bent until they start to crack, so that both the bending produced and its related moisture content are determined. However, this new version enables the calculation of PL from an equation, so it is not necessary to plot any curve or straight line to obtain this parameter and, in fact, the PL can be achieved with only one experimental point (but two experimental points are recommended).
The PL results obtained with this new version are very similar to those obtained through the original bending test and the standard rolling test by a highly experienced operator. Only in particular cases of high plasticity cohesive soils, there is a greater difference in the result. Despite this, the bending test works very well for all types of soil, both cohesive and very low plasticity soils, where the latter are the most difficult to test via the standard thread rolling method.

The traditional standardized test for determining the plastic limit in soils is performed by hand, and the result varies depending on the operator. An alternative method based on bending measurements is presented in this study. This allows the plastic limit to be obtained with a clear and objective criterion.

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

Material corrosion can be a limiting factor for different materials in many applications. Thus, it is necessary to better understand corrosion processes, prevent them and minimize the damages associated with them. One of the most important characteristics of corrosion processes is the corrosion rate. The measurement of corrosion rates is often very difficult or even impossible especially in less conductive, non-aqueous environments such as biofuels. Here, we present five different methods for the determination of corrosion rates and the efficiency of anti-corrosion protection in biofuels: (i) a static test, (ii) a dynamic test, (iii) a static test with a reflux cooler and electrochemical measurements (iv) in a two-electrode arrangement and (v) in a three-electrode arrangement. The static test is advantageous due to its low demands on material and instrumental equipment. The dynamic test allows for the testing of corrosion rates of metallic materials at more severe conditions. The static test with a reflux cooler allows for the testing in environments with higher viscosity (e.g., engine oils) at higher temperatures in the presence of oxidation or an inert atmosphere. The electrochemical measurements provide a more comprehensive view on corrosion processes. The presented cell geometries and arrangements (the two-electrode and three-electrode systems) make it possible to perform measurements in biofuel environments without base electrolytes that could have a negative impact on the results and load them with measurement errors. The presented methods make it possible to study the corrosion aggressiveness of an environment, the corrosion resistance of metallic materials, and the efficiency of corrosion inhibitors with representative and reproducible results. The results obtained using these methods can help to understand corrosion processes in more detail to minimize the damages caused by corrosion.

The testing of processes associated with material corrosion can often be difficult especially in non-aqueous environments. Here, we present different methods for short-term and long-term testing of corrosion behavior of non-aqueous environments such as biofuels, especially those containing bioethanol.

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

The whitefly Bemisia tabaci (Gennadius) is an invasive pest of considerable importance, affecting the production of vegetable and ornamental crops in many countries around the world. Severe yield losses are caused by direct feeding, and even more importantly, also by the transmission of more than 100 harmful plant pathogenic viruses. As for other invasive pests, increased international trade facilitates the dispersal of B. tabaci to areas beyond its native range. Inspections of plant import products at points of entry such as seaports and airports are, therefore, seen as an important prevention measure. However, this last line of defense against pest invasions is only effective if rapid identification methods for suspicious insect specimens are readily available. Because the morphological differentiation between the regulated B. tabaci and close relatives without quarantine status is difficult for non-taxonomists, a rapid molecular identification assay based on the loop-mediated isothermal amplification (LAMP) technology has been developed. This publication reports the detailed protocol of the novel assay describing rapid DNA extraction, set-up of the LAMP reaction, as well as interpretation of its read-out, which allows identifying B. tabaci specimens within one hour. Compared to existing protocols for the detection of specific B. tabaci biotypes, the developed method targets the whole B. tabaci species complex in one assay. Moreover the assay is designed to be applied on-site by plant health inspectors with minimal laboratory training directly at points of entry. Thorough validation performed under laboratory and on-site conditions demonstrates that the reported LAMP assay is a rapid and reliable identification tool, improving the management of B. tabaci.

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

This paper reports the protocol for a rapid identification assay for Bemisia tabaci based on loop-mediated isothermal amplification (LAMP) technology. The protocol requires minimal laboratory training and can, therefore, be implemented on-site at points of entry for plant imports such as seaports and airports.

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

Sample Preparation Method of Scanning and Transmission Electron Microscope for the Appendages of Woodboring Beetle

This report described sample preparation methods that scanning and transmission electron microscope observations, demonstrated by preparing appendages of the woodboring beetle, Chlorophorus caragana Xie &#38; Wang (2012), for both types of electron microscopy. The scanning electron microscopy (SEM) sample preparation protocol was based on sample chemical fixation, dehydration in a series of ethanol baths, drying, and sputter-coating. By adding Tween 20 (Polyoxyethylene sorbitan laurate) to the fixative and the wash solution, the insect body surface of woodboring beetle was washed more cleanly in SEM. This study&#39;s transmission electron microscopy (TEM) sample preparation involved a series of steps including fixation, ethanol dehydration, embedding in resin, positioning using fluorescence microscopy, sectioning, and staining. Fixative with Tween 20 enabled penetrate the insect body wall of woodboring beetle more easily than it would had been without Tween 20, and subsequently better fixed tissues and organs in the body, thus yielded clear transmission electron microscope observations of insect sensilla ultrastructures. The next step of this preparation was determining the positions of insect sensilla in the sample embedded in the resin block by using fluorescence microscopy to increase the precision of target sensilla positioning. This improved slicing accuracy.

In order to observe ultrastructure of insect sensilla, scanning and transmission electron microscopy (SEM and TEM, respectively) sample preparation protocol were presented in the study. Tween 20 was added into the fixative to avoid sample deformation in SEM. Fluorescence microscopy was helpful for improving slicing accuracy in TEM.

This report described sample preparation methods that scanning and transmission electron microscope observations, demonstrated by preparing appendages of ...