This material is based upon work supported by the U.S. Department of Homeland Security under Grant Award Number 2010-ST-061-FD0001 through a grant awarded by the National Center for Food Protection and Defense at the University of Minnesota. Disclaimer: The views and conclusions contained in this document are those of the authors and should not be interpreted as necessarily representing the official policies, either expressed or implied, of the U.S. Department of Homeland Security or the National Center for Food Protection and Defense.

1. Silbernanopartikelsynthese 15 <ol><li> Man löst 18 mg Silbernitrat in 100 ml Reinstwasser (18.2 ΩU) und Vortex für 5 Sek. </li><li> Man löst 27 mg Natriumzitratdihydrat in 1 ml Wasser und Vortex für 5 Sek. </li><li> Übertragen Sie alle der hergestellten Silbernitratlösung zu einem Erlenmeyerkolben mit Rührstab und stellte die Flasche auf einem Magnet heißen Platte enthält. Wird der Kolben unter kräftigem Rühren mit einer Rührgeschwindigkeit von 700 Umdrehungen pro Minute bei ~ 350 ° C (Einstellung Temperatur auf der Platte). </li><li> Beim Kochen, fügen sofort alle der vorbereiteten Natriumcitratlösung zu den Erlenmeyerkolben gegeben und die Lösung verlassen für weitere 25 min zum Sieden, bis die Lösung grünlich braun wird, die die Bildung von Ag-Nanopartikeln zeigt. </li><li> Entfernen Sie den Kolben von der heißen Platte und legen Sie sie auf einem anderen Magnetplatte (nicht erhitzen) und rühren O / N in der gleichen Rührgeschwindigkeit bei RT, bis die Mischung erreicht einen stabilen Zustand, mit einer konstanten Farbe und Transparency. Verwenden Sie ein UV-VIS-Spektrometer der Absorption der hergestellten Silber-Nanopartikel, um festzustellen, wenn nötig. </li><li> Verdünne die Endmischung mit ultrareinem Wasser auf 100 ml. </li><li> Verwenden Sie einen Zetasizer die Größe der Silber-Nanopartikel zu messen, wenn notwendig, nach dem Protokoll des Herstellers. </li><li> Übertragen Sie die Ag-Kolloid zu einem verschlossenen Behälter und schützen sie vor Licht mit Aluminiumfolie. Das Kolloid kann bei Bedarf für 2 Monate bei 4-7 ° C im Kühlschrank aufbewahrt werden. </li></ol> 2. Herstellung eines SERS Aktive Filter Membrane <ol><li> Man löst 2,92 g Natriumchlorid (NaCl) in 100 ml Wasser, um eine 50 mM NaCl-Lösung herzustellen. </li><li> 1 ml der 5 mM NaCl-Lösung in 1 ml der hergestellten Silber-Nanopartikel und mischen sie auf einem Taumelmischer für 10 Minuten bei 20 Umdrehungen pro Minute. Dieser Schritt ist die Silber-Nanopartikel in Ag-Nanocluster zu aggregieren. </li><li> Platzieren einer Filtermembran (PVDF, 0,1 um Porengrße) in einem Filterhalter, die an einer Spritze befestigt werden kann. Der kleinere Porengröße Membran war found wirksamer als die größere Porengröße Membran (dh 0,22 um) in Trapping Ag-Nanocluster und Erzeugen konsistenter Signale. </li><li> Last 2 ml der hergestellten Ag-Nanocluster in die Spritze für die Filtration. Bringen Sie den Filterhalter an der Spritze und manuell das gesamte Volumen von Ag-Nanocluster durch die Membran in einer Fließrate von 1 Tropfen / s übergeben. Die Membran Fallen Ag-Nanocluster, eine SERS-aktiven Filtermembran bilden. </li><li> Nehmen Sie die Filtermembran aus dem Filterhalter. Besondere Vorsicht ist geboten, wenn die Membran am äußeren Rand, die eine Pinzette keine Beschädigung der Membran zu gewährleisten. Luft trocknen für ca. 3 min und Platz Membran auf einem Glasträger. </li><li> Raman Detektion des SERS-Substrat <ol><li> Stellen Sie die Raman Instrument zu einem 780 nm Wellenlängenlaser mit einer Laserleistung von 5 mW, Bestrahlungszeit von 1 sec und Belichtungszahl von 2. Stellen Sie die mikroskopische Objektiv zu 10X. Stellen Sie sicher, das Ziel auf der Software entsprechend zu gesetzt ist. &lt;/ Li&gt; <li> Setzen Sie den Glasobjektträger mit der Membran auf der Oberseite auf die Plattform des Raman-Instruments und verwenden das Mikroskop auf der Oberfläche der Membran zu konzentrieren. </li><li> Wähle zufällig 8-10 Flecken von der Membranoberfläche und das Instrument wird sie automatisch in Folge sammeln. Offene spektralen Daten im Hersteller-Software für die Analyse. </li></ol></li></ol> 3. Anwendung der Active Filter System SERS zum Nachweis chemischer Kontaminanten <ol><li> Bereiten Sie eine 10 ppb Ferbam Lösung. Achtung: Ferbam ist sehr volatil. Vorsichtsmaßnahmen (Atemschutzmaske und Schutzbrille), wenn die feste wiegen. <ol><li> Wiegen Sie 2 mg Ferbam Pulver und löst ihn in 20 ml 50% Acetonitril (10 ml Acetonitril und 10 ml Wasser), um eine Stammlösung (100 ppm) zu machen. Mischen Sie den Kolben für 30 Sekunden. </li><li> Nehmen Sie 1 ml der 100 ppm Ferbam Lösung in einem Reagenzglas und fügen 9 ml 50% Acetonitril 10 ppm-Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li><li> Nehmen Sie 1 ml der10 ppm Lösung in einem Reagenzglas und fügen 9 ml 50% Acetonitril eine 1 ppm-Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li><li> Nehmen Sie 1 ml der 1 ppm Lösung in einem Reagenzglas und fügen 9 ml 50% Acetonitril eine 100-ppb-Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li><li> Nehmen Sie 1 ml der 100-ppb-Lösung in einem Reagenzglas und fügen 9 ml 50% Acetonitril 10 ppb Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li></ol></li><li> Bereiten Sie eine 1 ppm Ampicillin Lösung. <ol><li> Wiegen 10 mg Ampicillin Pulver und löst ihn in 100 ml Wasser auf 100 ppm Ampicillin-Lösung zu machen. Mischen Sie den Kolben für 30 Sekunden. </li><li> Nehmen Sie 1 ml der 100 ppm-Lösung in einem Reagenzglas und fügen 9 ml Wasser zu einer 10 ppm Ampicillin-Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li><li> Nehmen Sie 1 ml der 10-ppm-Lösung in einem Reagenzglas und fügen 9 ml Wasser zu einer 1 ppm Ampicillin-Lösung zu machen. Mischen Sie den Schlauch für 5 Sek. </li></ol></li><li> Setzen Sie die Filtermembran zurück in den Filterhalter, mit dem NP beschichtete Seite nach oben zeigt. &lt;/ Li&gt; <li> Last 5 ml einer Probe in eine neue Spritze, und dann hängen Sie es an den Filterhalter mit einer Ag-beschichtete Membran im Inneren. </li><li> geben manuell das gesamte Volumen der Probe durch die Membran in einer Fließrate von 1 Tropfen / s. Zielmoleküle können auf den auf der Filtermembran beschichteten Nanopartikeln adsorbiert und konzentriert werden. </li><li> Trennen Filtermembran aus dem Filterhalter, der Luft trocknen lassen für etwa 3 min und Messen der Signale des Raman-Instrument unter Verwendung der gleichen Methode wie in Schritt 2.6 beschrieben. </li><li> Wiederholen Sie Schritt 2,2 bis 2,6, um eine weitere Ag-beschichteten Membran vor, und ergeben sich aus Schritt 3.3 für den Nachweis der anderen Probe. </li></ol>

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The authors have nothing to disclose.

Einer der kritischen Schritte in diesem Protokoll ist das Silber-Nanopartikel-Synthese, wo gleichmäßige Silber-Nanopartikel der Schlüssel für konsistente Ergebnisse sind. Die Erwärmungszeit und die Konzentrationen von Vorstufen werden müssen präzise gesteuert. Die durchschnittliche Größe von 80 nm AGNPS Zubereitung ist, die durch die Zetasizer gemessen wurde (Daten nicht gezeigt). Ein weiterer kritischer Schritt ist das Salz Aggregation, wo die Salzkonzentration und Aggregationszeit müssen genau gesteuert werd...

Oberflächenverstärkten Raman-Spektroskopie (SERS) ist eine Technik, die Kombination von Raman-Spektroskopie mit Nanotechnologie. Die Intensität der Raman-Streuung von Analyten an Edelmetallnano Oberflächen wird durch die lokalisierte Oberflächenplasmonenresonanz stark verbessert. 1 Silber-Nanopartikel (Ag NPs) sind bei weitem die am häufigsten verwendeten SERS Substrate aufgrund seiner hohen Verstärkung Fähigkeit. 2 Bisher wurden verschiedene Syntheseverfahren von Ag-NPs entwickelt. 3-6 Ag-Nanopartikeln allein so wirksam SERS Substrate verwendet werden können, oder mit anderen Materialien und Strukturen kombiniert, um die Empfindlichkeit und / oder Funktionalität zu verbessern. 7-11 SERS-Techniken haben große Kapazität für die Detektion verschiedener Spurenmengen von Kontaminanten in Lebensmitteln und Umweltproben zeigten 12 Traditionell gibt es zwei allgemeine Möglichkeiten zur Herstellung eines SERS Beispiel:.. Lösungs-und-Substrat-basierte Verfahren 13 Die Lösungs-method verwendet NP Kolloide mit Proben zu mischen. Dann wird das NP-Analyt-Komplexes unter Verwendung von Zentrifugation gesammelt und auf einem festen Träger für die Raman-Messung nach dem Trocknen aufgebracht. Das Substrat-basierten Verfahren wird in der Regel durch Aufbringen von mehreren Mikroliter einer flüssigen Probe auf die vorgefertigte feste Substrat aufgebracht. 14 sind jedoch keine dieser beiden Methoden effektiv und geeignet für eine große Menge an Probenvolumen. Mehrere Änderungen der SERS-Assays überwand die Volumengrenzen, wie die Integration eines Filtersystems 15-21 oder den Einbau einer Mikrofluidik-Vorrichtung. 21-24 Die modifizierten SERS-Assays große Verbesserung in der Empfindlichkeit und Machbarkeit gezeigt haben, für die chemische Verunreinigungen Überwachung in großen Wasserproben. Hier zeigen wir die detaillierte Protokoll der Herstellung und Anwendung einer Spritzenfilter basierend SERS Verfahren Spurenmenge an Pestizid Ferbam und Antibiotikum Ampicillin zu detektieren.

<table border="0" cellpadding="0" cellspacing="0" width="604">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:211px;">Ampicillin</td>
			<td style="width:128px;">Fisher Scientific</td>
			<td style="width:136px;">BP1760-5</td>
			<td style="width:131px;">N/A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:211px;">Ferbam</td>
			<td style="width:128px;">Chem Service</td>
			<td style="width:136px;">N-11970-250MG</td>
			<td style="width:131px;">98+%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:211px;">Silver nitrate</td>
			<td style="width:128px;">Sigma Aldrich</td>
			<td style="width:136px;">209139</td>
			<td style="width:131px;">99.0+%</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:211px;">Sodium citrate dehydrate</td>
			<td style="width:128px;">Sigma Aldrich</td>
			<td style="width:136px;">W302600</td>
			<td style="width:131px;">99+%</td>
		</tr>
		<tr height="18">
			<td height="18" style="height:19px;width:211px;">Sodium chloride</td>
			<td style="width:128px;">Sigma Aldrich</td>
			<td style="width:136px;">S7653</td>
			<td style="width:131px;">99.5+%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:211px;">EMD Millipore Durapore PVDF Membrane Filters</td>
			<td style="width:128px;">Fisher Scientific</td>
			<td style="width:136px;">VVLP01300</td>
			<td style="width:131px;">0.10 &#181;m Pore Size, hydrophilic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:211px;">Polycarbonate Filter Holders</td>
			<td style="width:128px;">Cole-Parmer</td>
			<td style="width:136px;">EW-29550-40</td>
			<td style="width:131px;">13 mm diameter</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Analog Vortex Mixer</td>
			<td style="width:128px;">Fisher Scientific</td>
			<td>02-215-365</td>
			<td>N/A</td>
		</tr>
		<tr height="50">
			<td height="50" style="height:51px;width:211px;">Nutating Mixers</td>
			<td style="width:128px;">Fisher Scientific</td>
			<td>05-450-213</td>
			<td style="width:131px;">N/A</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:211px;">DXR Raman spectroscope</td>
			<td style="width:128px;">Thermo Scientific</td>
			<td style="width:136px;">IQLAADGABFFAHCMAPB</td>
			<td style="width:131px;">Laser power: 1 mW Exposure time: 5 s</td>
		</tr>
	</tbody>
</table>

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.

Die wichtigsten Schritte dieses Versuches wurden in der schematischen Darstellung (Abbildung 1). Abbildung 2 demonstriert die Bedeutung der optimierten Volumen AGNPS in der Membranbeschichtung zu verwenden, um die Empfindlichkeit maximiert zu erreichen. 1 ml der Silber-Nanopartikel bietet das stärkste Signal, wenn Ferbam verwenden, im Vergleich zu 0,5 ml (unzureichende Beschichtung) oder 2 ml (zuviel Beschichtung). <p class="jove_content" fo:keep-to...

Watch this Scientific Journal Video about A Filter-based Surface Enhanced Raman Spectroscopic Assay for Rapid Detection of Chemical Contaminants at JoVE.com

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

Ein Verfahren zur Herstellung und Durchführung der filterbasierten oberflächenverstärkten Raman-Spektroskopie (SERS) Assay zum Nachweis von chemischen Verunreinigungen (dh Pestizid Ferbam und Antibiotikum Ampicillin) dargestellt.

Ein Filter-basierten oberflächenverstärkter Raman-spektroskopische Assay zum schnellen Nachweis von chemischen Verunreinigungen

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

a-filter-based-surface-enhanced-raman-spectroscopic-assay-for-rapid

Research

JoVE Journal

Chemistry

9.3K Aufrufe.  University of Massachusetts Amherst.  Ein Verfahren zur Herstellung und Durchführung der filterbasierten oberflächenverstärkten Raman-Spektroskopie (SERS) Assay zum Nachweis von chemischen Verunreinigungen (dh Pestizid Ferbam und Antibiotikum Ampicillin) dargestellt. 

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

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

Herstellung von hydrophoben Metall-organische Gerüste über Plasma Enhanced Chemical Vapor Deposition von Perfluoralkanen für die Beseitigung von Ammoniak

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

Forschung

Chemie

A Simple and Rapid Protocol for Measuring Neutral Lipids in Algal Cells Using Fluorescence

Algae are considered excellent candidates for renewable fuel sources due to their natural lipid storage capabilities. Robust monitoring of algal fermentation processes and screening for new oil-rich strains requires a fast and reliable protocol for determination of intracellular lipid content. Current practices rely largely on gravimetric methods to determine oil content, techniques developed decades ago that are time consuming and require large sample volumes. In this paper, Nile Red, a fluorescent dye that has been used to identify the presence of lipid bodies in numerous types of organisms, is incorporated into a simple, fast, and reliable protocol for measuring the neutral lipid content of Auxenochlorella protothecoides, a green alga. The method uses ethanol, a relatively mild solvent, to permeabilize the cell membrane before staining and a 96 well micro-plate to increase sample capacity during fluorescence intensity measurements. It has been designed with the specific application of monitoring bioprocess performance. Previously dried samples or live samples from a growing culture can be used in the assay.

A simple protocol to determine the neutral lipid content of algal cells using a Nile Red staining procedure is described. This time-saving technique offers an alternative to traditional gravimetric-based lipid quantification protocols. It has been designed for the specific application of monitoring bioprocess performance.

Eine einfache und schnelle Protokoll zur Messung neutralen Lipiden in Algenzellen mit Fluoreszenz

Algae are considered excellent candidates for renewable fuel sources due to their natural lipid storage capabilities. Robust monitoring of algal ...

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

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

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

Vorbereitung hoch poröser Koordinationspolymerbeschichtungen auf makroporösen Monoliths für verbesserte Anreicherung von Phosphopeptiden

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

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

Eine Methode, die Oberflächenspannung eines Liquid Metal manipulieren via Oberfläche Oxidation und Reduktion

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Preparation of Biopolymer Aerogels Using Green Solvents

Although the first reports on aerogels made by Kistler1 in the 1930s dealt with aerogels from both inorganic oxides (silica and others) and biopolymers (gelatin, agar, cellulose), only recently have biomasses been recognized as an abundant source of chemically diverse macromolecules for functional aerogel materials. Biopolymer aerogels (pectin, alginate, chitosan, cellulose, etc.) exhibit both specific inheritable functions of starting biopolymers and distinctive features of aerogels (80-99% porosity and specific surface up to 800 m2/g). This synergy of properties makes biopolymer aerogels promising candidates for a wide gamut of applications such as thermal insulation, tissue engineering and regenerative medicine, drug delivery systems, functional foods, catalysts, adsorbents and sensors. This work demonstrates the use of pressurized carbon dioxide (5 MPa) for the ionic cross linking of amidated pectin into hydrogels. Initially a biopolymer/salt dispersion is prepared in water. Under pressurized CO2 conditions, the pH of the biopolymer solution is lowered to 3 which releases the crosslinking cations from the salt to bind with the biopolymer yielding hydrogels. Solvent exchange to ethanol and further supercritical CO2 drying (10 - 12 MPa) yield aerogels. Obtained aerogels are ultra-porous with low density (as low as 0.02 g/cm3), high specific surface area (350 - 500 m2/g) and pore volume (3 - 7 cm3/g for pore sizes less than 150 nm).

A new way for the production of biopolymer-based aerogels by carbon dioxide (CO2) induced gelation is shown. The technique utilizes pressurized carbon dioxide (5 MPa) for the production of biopolymer hydrogels and supercritical CO2 (12 MPa) to convert gels into aerogels. The only solvents needed besides CO2 are water and ethanol.

Herstellung von Biopolymer Aerogele unter Verwendung der grünen Lösungsmittel

Although the first reports on aerogels made by Kistler1 in the 1930s dealt with aerogels from both inorganic oxides (silica and others) and biopolymers ...

A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer

A novel approach for the Raman measurement of nuclear materials is reported in this paper. It consists of the enclosure of the radioactive sample in a tight capsule that isolates the material from the atmosphere. The capsule can optionally be filled with a chosen gas pressurized up to 20 bars. The micro-Raman measurement is performed through an optical-grade quartz window. This technique permits accurate Raman measurements with no need for the spectrometer to be enclosed in an alpha-tight containment. It therefore allows the use of all options of the Raman spectrometer, like multi-wavelength laser excitation, different polarizations, and single or triple spectrometer modes. Some examples of measurements are shown and discussed. First, some spectral features of a highly radioactive americium oxide sample (AmO2) are presented. Then, we report the Raman spectra of neptunium oxide (NpO2) samples, the interpretation of which is greatly improved by employing three different excitation wavelengths, 17O doping, and a triple mode configuration to measure the anti-stokes Raman lines. This last feature also allows the estimation of the sample surface temperature. Finally, data that were measured on a sample from Chernobyl lava, where phases are identified by Raman mapping, are shown.

We present a technique for Raman spectroscopic analysis of highly radioactive samples compatible with any standard micro-Raman spectrometer, without any radioactive contamination of the instrument. We also show some applications using actinide compounds and irradiated fuel materials.

Eine neue Technik für die Raman-Analyse von hochradioaktivem Proben jeden Standard Micro-Raman-Spektrometers

A novel approach for the Raman measurement of nuclear materials is reported in this paper. It consists of the enclosure of the radioactive sample in a ...

Observation and Analysis of Blinking Surface-enhanced Raman Scattering

From a single molecule at a silver nanoaggregate junction, blinking surface-enhanced Raman scattering (SERS) is observed. Here, a protocol is presented on how to prepare the SERS-active silver nanoaggregate, record a video of certain blinking spots in the microscopic image, and analyze the blinking statistics. In this analysis, a power law reproduces the probability distributions for bright events relative to their duration. The probability distributions for dark events are fitted by a power law with an exponential function. The parameters of the power law represent molecular behavior in both bright and dark states. The random walk model and the speed of the molecule across the entire silver surface can be estimated. It is difficult to estimate even when using averages, autocorrelation functions, and super-resolution SERS imaging. In the future, power law analyses should be combined with spectral imaging, because the origins of blinking cannot be confirmed by this analysis method alone.

This protocol describes the analysis of blinking surface-enhanced Raman scattering due to the random walk of a single molecule on a silver surface using power laws.

Beobachtung und Analyse der Oberfläche-enhanced Raman-Streuung zu blinken

From a single molecule at a silver nanoaggregate junction, blinking surface-enhanced Raman scattering (SERS) is observed. Here, a protocol is presented on ...

Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and other border protection agencies globally. Color testing is a presumptive identification technique indicating the presence or absence of a particular drug class using rapid and uncomplicated chemical methods. Owing to their relatively recent emergence, a color test for the specific identification of synthetic cathinones is not currently available. In this study, we introduce a protocol for the presumptive identification of synthetic cathinones, employing three aqueous reagent solutions: copper(II) nitrate, 2,9-dimethyl-1,10-phenanthroline (neocuproine) and sodium acetate. Small pin-head sized amounts (approximately 0.1-0.2 mg) of the suspected drugs are added to the wells of a porcelain spot plate, and each reagent is then added dropwise sequentially before heating on a hotplate. A color change from very light blue to yellow-orange after 10 min indicates the likely presence of synthetic cathinones. The highly stable and specific test reagent has the potential for use in the presumptive screening of unknown samples for synthetic cathinones in a forensic laboratory. However, the nuisance of an added heating step for the color change result limits the test to laboratory application and decreases the likelihood of an easy translation to field testing.

Here we present a simple, inexpensive, and selective chemical spot test protocol for the detection of synthetic cathinones, a class of new psychoactive substances. The protocol is suitable for use in various areas of law enforcement that encounter illicit material.

Vor Ort Farbtest als mutmaßlichen Werkzeug für die schnelle Erkennung von synthetischen Cathinone

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and ...

Gold Nanoparticle Modified Carbon Fiber Microelectrodes for Enhanced Neurochemical Detection

For over 30 years, carbon-fiber microelectrodes (CFMEs) have been the standard for neurotransmitter detection. Generally, carbon fibers are aspirated into glass capillaries, pulled to a fine taper, and then sealed using an epoxy to create electrode materials that are used for fast scan cyclic voltammetry testing. The use of bare CFMEs has several limitations, though. First and foremost, the carbon fiber contains mostly basal plane carbon, which has a relatively low surface area and yields lower sensitivities than other nanomaterials. Furthermore, the graphitic carbon is limited by its temporal resolution, and its relatively low conductivity. Lastly, neurochemicals and macromolecules have been known to foul at the surface of carbon electrodes where they form non-conductive polymers that block further neurotransmitter adsorption. For this study, we modify CFMEs with gold nanoparticles to enhance neurochemical testing with fast scan cyclic voltammetry. Au3+ was electrodeposited or dipcoated from a colloidal solution onto the surface of CFMEs. Since gold is a stable and relatively inert metal, it is an ideal electrode material for analytical measurements of neurochemicals. Gold nanoparticle modified (AuNP-CFMEs) had a stability to dopamine response for over 4 h. Moreover, AuNP-CFMEs exhibit an increased sensitivity (higher peak oxidative current of the cyclic voltammograms) and faster electron transfer kinetics (lower &#916;EP or peak separation) than bare unmodified CFMEs. The development of AuNP-CFMEs provides the creation of novel electrochemical sensors for detecting fast changes in dopamine concentration and other neurochemicals at lower limits of detection. This work has vast applications for the enhancement of neurochemical measurements. The generation of gold nanoparticle modified CFMEs will be vitally important for the development of novel electrode sensors to detect neurotransmitters in vivo in rodent and other models to study neurochemical effects of drug abuse, depression, stroke, ischemia, and other behavioral and disease states.

In this study, we modify carbon-fiber microelectrodes with gold nanoparticles to enhance the sensitivity of neurotransmitter detection.

Gold Nanopartikel Modifizierte Kohlenstofffaser-Mikroelektroden für verbesserte neurochemische Detektion

For over 30 years, carbon-fiber microelectrodes (CFMEs) have been the standard for neurotransmitter detection. Generally, carbon fibers are aspirated into ...

A Two-Step Pyrolysis-Gas Chromatography Method with Mass Spectrometric Detection for Identification of Tattoo Ink Ingredients and Counterfeit Products

Tattoo inks are complex mixtures of ingredients. Each of them possesses different chemical properties which have to be addressed upon chemical analysis. In this method for two-step pyrolysis online coupled to gas chromatography mass spectrometry (py-GC-MS) volatile compounds are analyzed during a first desorption run. In the second run, the same dried sample is pyrolyzed for analysis of non-volatile compounds such as pigments and polymers. These can be identified by their specific decomposition patterns. Additionally, this method can be used to differentiate original from counterfeit inks. Easy screening methods for data evaluation using the average mass spectra and self-made pyrolysis libraries are applied to speed up substance identification. Using specialized evaluation software for pyrolysis GS-MS data, a fast and reliable comparison of the full chromatogram can be achieved. Since GC-MS is used as separation technique, the method is limited to volatile substances upon desorption and after pyrolysis of the sample. The method can be applied for quick substance screening in market control surveys since it requires no sample preparation steps.

This method for two-step pyrolysis online coupled to gas chromatography with mass spectrometric detection and data evaluation protocol can be used for multi-component analysis of tattoo inks and discrimination of counterfeit products.

Eine zweistufte Pyrolysis-Gas-Chromatographie-Methode mit Massenspektrometrische Erkennung zur Identifizierung von Tattoo-Ink-Inhaltsstoffen und gefälschten Produkten

Tattoo inks are complex mixtures of ingredients. Each of them possesses different chemical properties which have to be addressed upon chemical analysis. ...