Die Arbeiten in diesem Papier beschrieben wurden durch einen Zuschuss von den CII-HK / PolyU Innovationsfonds unterstützt. Weitere Unterstützung wurde von dem Shenzhen Peacock Plan (KQTD2015071616442225) und die chinesischen Regierung &quot;Thousand Talent&quot; Program (Y62HB31601) zur Verfügung gestellt. Auch die Hilfe von der Abteilung für angewandte Biologie &amp; Chemical Technology von der Hong Kong Polytechnic University und der Hong Kong Polytechnic University Research Institute für nachhaltige Stadtentwicklung (RISUD) geschätzt wird.

1. Vorbehandlung von HGM <ol><li> Platzieren Sie die HGM in ein 500-ml-Becherglas mit 200 ml absolutem Alkohol; Die geringe Dichte des ungebrochenen HGM verursacht es in dem Alkohol zu unterbrechen, sondern weil die Dichte von gebrochenem HGM größer ist als diejenige von Alkohol, fällt es in der Lösung. Nach 30 min sammeln bei 80 ° C in einem Ofen für eine weitere Anwendung des suspendierten HGM mit einem sauberen Löffel und trocken. </li></ol> 2. Synthese von MCHGM <ol><li> Place 5 g ungebrochen HGM, 47,5 ml Ethanol und 2,5 ml DI-Wasser in einem Dreihalskolben. Rühre einen Rührmotor Verwendung bei 400 r / min für 20 min (Vormischen). </li><li> Mix 15 g TBT wurden 1 g PFOTES und 30 ml absolutem Alkohol in einem 200 ml - Becherglas gegeben. Die Mischung wurde in einem Konstantdruck-Trichter. </li><li> Legen der Konstantdruck Trichter in eine der Öffnungen des Dreihalskolben. Drop die Mischung in der Konstantdruck Trichter in den Dreihalskolben mit einer Geschwindigkeit von enthaltenen1 Tropfen pro 7 s, die durch Einstellen des Ventils des Konstantdruckrichters erreicht wird. Weiter die Reaktion für 3 Stunden. </li><li> Die Mischung aus dem Dreihalskolben in einen hydrothermalen Reaktor. Setzen Sie den versiegelten Reaktor in einer geeigneten Stahlhülse in einem 180 ° C-Ofen für 6 h. HINWEIS: Stellen Sie sicher, dass der Reaktor eine geeignete Abdeckung hat. Nachdem es bedeckt ist, setzte den Reaktor in die Stahlhülse. Die Hülse ist auch mit einem Deckel verschlossen werden. </li><li> Nachdem die Reaktion vorbei ist, sammeln die in dem hydrothermalen Reaktor suspendiert Proben einen großen Löffel. Trocknen Sie die Proben bei 80 ° C für 4 h MCHGM zu erhalten. </li></ol> 3. Synthese von F-SCHGM <ol><li> 5 g ungebrochen HGM, 47,5 ml absoluten Ethanol und 2,5 ml DI-Wasser in einen Dreihalskolben. Rühre einen Rührmotor Verwendung bei 400 r / min für 20 min (Vormischen). Mix 1 g PFOTES und 30 ml absoluten Ethanol in einem 200 ml - Becherglas gegeben. Übertragen Sie die PFOTES und absolute eTHANOL Mischung auf einen Konstantdruck-Trichter. </li><li> Legen der Konstantdruck Trichter in den Dreihalskolben. Drop die Mischung in dem Konstantdruck Trichtern in die Dreihalskolben mit einer Geschwindigkeit von 1 Tropfen pro s 7 enthalten. Lassen Sie die Reaktion 3 h laufen. </li><li> Übertragen die Mischung aus dem Dreihalskolben, einen hydrothermischen Reaktor. Setzen Sie den verschlossenen Reaktor in einem 180 ° C-Ofen für 6 h. Nachdem die Reaktion vorbei ist, sammeln die in dem hydrothermalen Reaktor suspendiert Proben einen großen Löffel. Trocknen Sie die Proben bei 80 ° C für 4 h F-SCHGM zu erhalten. </li></ol> 4. Synthese von Ti-SCHGM <ol><li> Place 5 g ungebrochen HGM, 47,5 ml absoluten Ethanol und 2,5 ml DI-Wasser in einem Dreihalskolben. Rühre bei 400 r / min für 20 min (Vormischen). Mix 15 g TBT und 30 ml absoluten Ethanol in einem 200 ml - Becherglas gegeben. Übertragen des TBT und absoluten Ethanol-Gemisches mit einem Konstantdruck-Trichter. </li><li> Legen Sie die Konstante-pressicher Trichter in den Dreihalskolben. Drop die Mischung in dem Konstantdruck Trichter in die Dreihalskolben mit einer Geschwindigkeit von 1 Tropfen pro 7 s. Lassen Sie die Reaktion 3 h laufen. </li><li> Übertragen die Mischung aus dem Dreihalskolben, einen hydrothermischen Reaktor. Setzen Sie den verschlossenen Reaktor in einem 180 ° C-Ofen für 6 h. Sammeln Sie die Proben in dem hydrothermalen Reaktor, nachdem die Reaktion beendet ist. Trocknen Sie die Proben bei 80 ° C für 4 h Ti-SCHGM zu erhalten. </li></ol> 5. Charakterisierungen <ol><li> Führen XRD Charakterisierungen auf allen Proben. Sammeln Sie die Daten ein sehr vielseitiges Mehrzweckröntgenbeugungssystem mit Cu K &amp; alpha; Strahlung (λ = 0,15406 nm) und einem 2θ von 10 ° bis 80 ° reichen. </li><li> Acquire Rasterelektronenmikroskops 20, 21 Bilder , nachdem die Proben mit Gold - Sprühen. Während der REM-Tests führen die EDS auf einen bestimmten Bereich ist. </li><li> Messen Sie dieKontaktwinkel durch einen Kontaktwinkel - Goniometer unter Verwendung von 22; die Wassertropfenvolumen sollte 10 &amp; mgr; l sein. </li><li> Misst den Gleitwinkel 23 durch den Neigungswinkel der Oberfläche zu verändern. Minimieren Sie den Winkel, bis der Wassertropfen nach unten nur gleiten kann. <ol><li> Haften doppelseitiges Klebeband auf einer Glasplatte (Grße: 26 mm x 76 mm x 2 mm). Mit einem Löffel, legt gleichmäßig um die Pulver (F-SCHGM oder MCHGM) auf dem Band. Verwendung eines Injektors, fügen einen Wassertropfen (Volumen: 0,05 ml) zu der Pulveroberfläche. </li><li> Setzen Sie die Glasscheibe auf der Motorplattform des Kontaktwinkel-Goniometer. Neigen der Glasscheibe, indem er sich die Motorplattform mit einer Rate von 1 ° / s. Stoppen Sie den Motor, wenn der Wassertropfen zu rutschen beginnt; der Neigungswinkel ist der Gleitwinkel. </li></ol></li><li> Messen Sie die Reflexionsspektren mit einem Spektralphotometer 24. HINWEIS: Die Wellenlänge von 450 nm bis 2.550 nm. </li><li> Messung der thermischen Leitfähigkeit aller Probenunter Verwendung eines thermischen Leitfähigkeitsmessgerät 25. </li></ol>

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The authors have nothing to disclose.

In diesem Manuskript ist der kritische Schritt in dem Protokoll die hydrothermalen Verfahren. Es beeinflusst die Bildung von TiO 2, die letzten Reflexionsvermögen und die superhydrophoben. Die Temperaturkontrolle und Reaktionszeit ist auch sehr wichtig. Wenn die Reaktionsbedingungen zu ändern, können die Endprodukte fehlerhaft sein. Diese Methode bietet einen einfachen Weg superhydrophoben und hoch IR-reflektierenden HGM in einem Schritt zu synthetisieren. In früheren Forschun...

Hohlglasmikrokugeln (HGM) sind anorganische Materialien in der Größe im Bereich von 10 bis 100 um. Sie zeigen viele nützlichen Eigenschaften, wie ausgezeichnete Dispersion, hohe Fließfähigkeit, geringe Dichte und hervorragende Wärmeisoliereigenschaften 1, 2, 3, 4. Aufgrund ihrer Hohlstruktur hat HGM eine extrem niedrige Wärmeleitfähigkeit 10, 11. Aus diesen Gründen werden sie in vielen Bereichen angewandt, einschließlich der Luft- und Raumfahrt 5, Tiefsee-Exploration 6, 7, Wasserstoffspeicher 8, 9, usw. Aber sie immer noch einige Nachteile, wie geringe Festigkeit aufweisen. Darüber hinaus ist das IR-Licht in der Lage durch HGM zu übertragen und das Thema hinter beheizen. dafüre, Oberflächenmodifikationen auf HGM sind unerlässlich, um die Strahlungswärmeübertragung zu reduzieren. Eine wirksame Methode ist die Beschichtung ein IR-blockierende Material auf die Oberfläche HGM. Als Halbleiter hat TiO 2 16 in vielen Bereichen, wie beispielsweise das Photokatalyse 12, 13, Solarzellen Entwicklung, Fertigung Sensor 14, Umweltanwendungen 15 und Energiespeicher verwendet. Darüber hinaus zeigt sie auch mit geringem Emissionsvermögen im sichtbaren Licht und Infrarotband 17, 18, 19. Daher ist für unsere Zwecke war TiO 2 eine umsichtige Auswahl aufgrund seiner relativ niedrigen Preis und hoher Leistung. Allerdings ist die Beschichtung ganz einfach für Schadstoffe zu beschmutzen, die ernsthaft die Reflektivität von TiO 2 wirkt. Das Reflexionsvermögen muss nach und nach reduzieren. Daher ist ein self reinigende Beschichtung ist wichtig, die Beschichtung vor Verschmutzung zu verhindern und die Arbeitszeit einer solchen Beschichtung zu verlängern. In diesem Manuskript wurde ein Soft-Chemie verwendetes Verfahren superhydrophoben TiO 2 -beschichteten HGM zu entwickeln. Tetrabutyltitanat (TBT) und 1H, 1H, 2H, 2H-Perfluoroctyltriethoxysilan (PFOTES) wurden als Ti-Quelle und superhydrophoben Mittel ausgewählt sind. Sie wurden auf der HGM Oberfläche hydrolysiert und abgeschieden. Dann, nach dem hydrothermalen Verfahren, der Anatas - TiO 2 auf der HGM Oberfläche gebildet, und die superhydrophobe Eigenschaften blieben. Zum Vergleich PFOTES einfach beschichteten HGM (F-SCHGM) und TiO 2 einfach beschichteten HGM (Ti-SCHGM) wurden ebenfalls synthetisiert. Das Syntheseschema ist in Abbildung 1 dargestellt.

<table border="0" cellpadding="0" cellspacing="0" width="471">
	<tbody>
		<tr height="19">
			<td height="19" style="height:19px;width:207px;">HGM</td>
			<td style="width:88px;">Technical Institute of Physics and Chemistry, Chinese Academy of Science</td>
			<td style="width:88px;">N/A</td>
			<td style="width:88px;">N/A</td>
		</tr>
		<tr height="19">
			<td height="19" style="height:19px;">TBT</td>
			<td>Sigma-Aldrich</td>
			<td>CAS#: 5593-70-4</td>
			<td>Analytical grade</td>
		</tr>
		<tr height="19">
			<td height="19" style="height:19px;">Ethyl Alcohol</td>
			<td>Sigma-Aldrich</td>
			<td>CAS#: 64-17-5</td>
			<td>Analytical grade</td>
		</tr>
		<tr height="19">
			<td height="19" style="height:19px;">PFOTES</td>
			<td>Sigma-Aldrich</td>
			<td>CAS#: 51851-37-7</td>
			<td align="right">98%</td>
		</tr>
	</tbody>
</table>

tio2-coated hollow glass microspheres with superhydrophobic and high ir-reflective properties synthesized by a soft-chemistry method

Diese Handschrift schlägt vor, ein Soft-Chemie Verfahren superhydrophoben und hoch IR-reflektierenden Glasmikrohohlkugeln (HGM) zu entwickeln. Die Anatas - TiO 2 und ein superhydrophobe Mittel wurden in einem Arbeitsgang auf der HGM beschichtende Oberfläche. TBT und PFOTES wurden als Ti-Quelle und der superhydrophoben Mittel jeweils ausgewählt. Sie wurden beide auf dem HGM beschichtet, und nach dem hydrothermalen Verfahren, das TBT gedreht TiO 2 Anatas. Auf diese Weise wird ein PFOTES / TiO 2 -beschichteten HGM (MCHGM) wurde hergestellt. Zum Vergleich PFOTES einfach beschichteten HGM (F-SCHGM) und TiO 2 einfach beschichteten HGM (Ti-SCHGM) wurden ebenfalls synthetisiert. Das PFOTES und TiO 2 -Beschichtungen auf der HGM Oberfläche wurden durch Röntgenbeugung (XRD), Rasterelektronenmikroskopie (SEM) und energiedispersiver Detektor (EDS) Charakterisierungen demonstriert. Die MCHGM zeigte einen höherer Kontaktwinkel (153 °), aber einen niedrigeren Gleitwinkel (16 °) als F-SCHGM, mit einem Kontaktwinkel von 141,26; und einen Gleitwinkel von 67 °. Zusätzlich zeigten beide Ti-SCHGM und MCHGM Ähnliche IR-Reflexionswerte, die etwa 5,8% höher als die ursprüngliche HGM und F-SCHGM waren. Außerdem änderte sich die PFOTES Beschichtung kaum die Wärmeleitfähigkeit. Daher F-SCHGM, mit einer Wärmeleitfähigkeit von 0,0479 W / (m · K), war ganz wie das Original HGM, das 0,0475 W / (m · K) war. MCHGM und Ti-SCHGM waren ebenfalls ähnlich. Deren Wärmeleitfähigkeitswerte waren 0,0543 W / (m · K) und 0,0543 W / (m · K), respectively. Die TiO 2 -Beschichtung leicht erhöhte die thermische Leitfähigkeit, aber mit der Erhöhung der Reflektivität wurde die Gesamtwärmeisolationseigenschaft verbessert. Schließlich, da die IR-reflektierende Eigenschaft von der HGM Beschichtung versehen ist, wenn die Beschichtung verschmutzt ist, verringert sich die Reflektivität. Daher kann mit der superhydrophoben Beschichtung wird die Oberfläche vor Verschmutzung geschützt, und ihre Lebensdauer ist auch verlängert.

Die Tests in Schritt 4.4 zeigen viele Merkmale und Eigenschaften der Proben. Die XRD (Figur 2) gibt die Bildung von Anatas - TiO 2. Die SEM (Abbildung 3) und EDS (Figur 4) zeigt das TiO 2 und die auf der PFOTES HGM Oberfläche beschichtet sind. Der Kontaktwinkel (Abbildung 5) und Schiebewinkel (Abbildung 6) Tests stellen die Superhydrophobie. Der VIS-NIR -Durchlässigkeitstest <stro...

Watch this Scientific Journal Video about TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method at JoVE.com

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

TiO<sub&gt; 2</sub&gt; -beschichteten Glashohlkugeln mit Superhydrophobe und hohe IR-reflektierende durch eine Soft-Chemie synthetisiert Eigenschaften

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

tio2-coated-hollow-glass-microspheres-with-superhydrophobic-high-ir

Research

JoVE Journal

Chemistry

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

10.0K Aufrufe.  City University of Hong Kong. This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

Serie: TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, 1,4-benzene-bis(iminoguanidinium) (BBIG), is demonstrated. The ligand is synthesized as the chloride salt (BBIG-Cl) by in situ imine condensation of terephthalaldehyde with aminoguanidinium chloride in water, followed by crystallization as the sulfate salt (BBIG-SO4). Alternatively, BBIG-Cl is synthesized ex situ in larger scale from ethanol. The sulfate separation ability of the BBIG ligand is demonstrated by selective and quantitative crystallization of sulfate from seawater. The ligand can be recycled by neutralization of BBIG-SO4 with aqueous NaOH and crystallization of the neutral bis-iminoguanidine, which can be converted back into BBIG-Cl with aqueous HCl and reused in another separation cycle. Finally, 35S-labeled sulfate and &#946; liquid scintillation counting are employed for monitoring the sulfate concentration in solution. Overall, this protocol will instruct the user in the necessary skills to synthesize a ligand, employ it in the selective crystallization of sulfate from aqueous solutions, and quantify the separation efficiency.

A protocol for in situ aqueous synthesis of a bis(iminoguanidinium) ligand and its utilization in selective separation of sulfate is presented.

Sulfate Trennung durch selektive Kristallisation mit einer Bis-iminoguanidinium Ligand

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, ...

Forschung

Chemie

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

Synthese und Charakterisierung von Fe-dotierten Aluminosilikatgerüststoffe Nanoröhrchen mit Enhanced Electron leitenden Eigenschaften

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC)

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil quality, food flavoring, and human health. The biological activity of glucosinolates is released upon tissue damage, when they are mixed with the enzyme myrosinase. This results in the formation of pungent and toxic breakdown products, such as isothiocyanates and nitriles. Currently, more than 130 structurally different glucosinolates have been identified. The chemical structure of the glucosinolate is an important determinant of the product that is formed, which in turn determines its biological activity. The latter may range from detrimental (e.g., progoitrin) to beneficial (e.g., glucoraphanin). Each glucosinolate-containing plant species has its own specific glucosinolate profile. For this reason, it is important to correctly identify and reliably quantify the different glucosinolates present in brassicaceous leaf, seed, and root crops or, for ecological studies, in their wild relatives. Here, we present a well-validated, targeted, and robust method to analyze glucosinolate profiles in a wide range of plant species and plant organs. Intact glucosinolates are extracted from ground plant materials with a methanol-water mixture at high temperatures to disable myrosinase activity. Thereafter, the resulting extract is brought onto an ion-exchange column for purification. After sulfatase treatment, the desulfoglucosinolates are eluted with water and the eluate is freeze-dried. The residue is taken up in an exact volume of water, which is analyzed by high-pressure liquid chromatography (HPLC) with a photodiode array (PDA) or ultraviolet (UV) detector. Detection and quantification are achieved by conducting comparisons of the retention times and UV spectra of commercial reference standards. The concentrations are calculated based on a sinigrin reference curve and well-established response factors. The advantages and disadvantages of this straightforward method, when compared to faster and more technologically advanced methods, are discussed here.

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography HPLC

Here, we describe in great detail an established and robust protocol for the extraction of glucosinolates from ground plant materials. After an on-column sulfatase treatment of the extracts, the desulfoglucosinolates are eluted and analyzed by high-pressure liquid chromatography.

Eine einfache Methode zur Glucosinolate Extraktion und Analyse mit Hochdruck-Flüssigkeitschromatographie (HPLC)

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil ...

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and related diseases, but their precise measurement is still a challenge. Many protocols have been described for neurotransmitter measurement by a variety of instruments, including high-pressure liquid chromatography (HPLC). However, there are shortcomings, such as complicated operation or hard-to-detect multiple targets, which cannot be avoided, and presently, the dominant analysis technique is still HPLC coupled with sensitive electrochemical or fluorimetric detection, due to its high sensitivity and good selectivity. Here, a detailed protocol is described for the pretreatment and detection of catecholamines with high pressure liquid chromatography with electrochemical detection (HPLC-ECD) in real urine samples of infants, using electrospun composite nanofibers composed of polymeric crown ether with polystyrene as adsorbent, also known as the packed-fiber solid phase extraction (PFSPE) method. We show how urine samples can be easily precleaned by a nanofiber-packed solid phase column, and how the analytes in the sample can be rapidly enriched, desorbed, and detected on an ECD system. PFSPE greatly simplifies the pretreatment procedures for biological samples, allowing for decreased time, expense, and reduction of the loss of targets. 
Overall, this work illustrates a simple and convenient protocol for solid-phase extraction coupled to an HPLC-ECD system for simultaneous determination of three monoamine neurotransmitters (norepinephrine (NE), epinephrine (E), dopamine (DA)) and two of their metabolites (3-methoxy-4-hydroxyphenylglycol (MHPG) and 3,4-dihydroxy-phenylacetic acid (DOPAC)) in infants' urine. The established protocol was applied to assess the differences of urinary catecholamines and their metabolites between high-risk infants with perinatal brain damage and healthy controls. Comparative analysis revealed a significant difference in urinary MHPG between the two groups, indicating that the catecholamine metabolites may be an important candidate marker for early diagnosis of cases at risk for brain damage in infants.

We present a convenient solid-phase extraction coupled to high-pressure liquid chromatography (HPLC) with electrochemical detection (ECD) for simultaneous determination of three monoamine neurotransmitters and two of their metabolites in infants' urine. We also identify the metabolite MHPG as a potential biomarker for the early diagnosis of brain damage for infants.

Eine bequeme Methode für die Extraktion und Analyse mit Hochdruck-Flüssigkeitschromatographie Katecholamin Neurotransmitter und deren Metabolite

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and ...

Preparation of Hollow Polystyrene Particles and Microcapsules by Radical Polymerization of Janus Droplets Consisting of Hydrocarbon and Fluorocarbon Oils

In this article, we have demonstrated a method for producing hollow particles and microcapsules using oil droplets consisting of hydrocarbon oil (styrene) and fluorocarbon oil (perfluoro-n-octane, PFO) in aqueous surfactant (sodium dodecylsulfate, SDS) solutions. Since fluorocarbon oils are immiscible with hydrocarbon oils, the two oils are separated. Emulsions are prepared by stirring styrene/PFO/aqueous SDS solution mixtures at 80 &#176;C. The type of emulsions and the morphology of droplets in the emulsions are observed by light microscope and scanning confocal fluorescence microscope. It is found that oil droplets with Janus-type morphologies consisting of mutually immiscible styrene and PFO are formed in aqueous SDS solutions. Polystyrene particles are fabricated by radical polymerization of the ternary mixtures of styrene/PFO/aqueous SDS solution at 80 &#176;C. The morphologies of the polystyrene are confirmed by scanning electron microscopy and scanning transmission electron microscopy observations. These observations show the preparation of hollow polystyrene particles with a single hole on the surface. To our knowledge, this method is a novel strategy using the immiscibility of hydrocarbon and fluorocarbon oils. The hollow particles can also be applied to the preparation of microcapsules.

A protocol for the fabrication of hollow polymer particles and microcapsules by radical polymerization using emulsions consisting of styrene, perfluoro-n-octane, and aqueous SDS (sodium dodecylsulfate) solution is presented.

Vorbereitung der hohlen Polystyrol Partikel und Mikrokapseln durch radikalische Polymerisation von Janus Tröpfchen bestehend aus Kohlenwasserstoff und Fluorcarbon-Öle

In this article, we have demonstrated a method for producing hollow particles and microcapsules using oil droplets consisting of hydrocarbon oil (styrene) ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Chemischen Niederschlag-Methode für die Synthese von Nb2O5 geändert, Bulk-Nickel-Katalysatoren mit hoher spezifischer Oberfläche

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to diversify the fiber choices in the United States body armor market, copolymer fibers based on the combination of 5-amino-2-(p-aminophenyl) benzimidazole (PBIA) and the more conventional PPTA were introduced. Little is known regarding the long-term stability of these fibers, but as condensation polymers, they are expected to have potential sensitivity to moisture and humidity. Therefore, characterizing the strength of the materials and understanding their vulnerability to environmental conditions is important for evaluating their use lifetime in safety applications. Ballistic resistance and other critical structural properties of these fibers are predicated on their strength. To accurately determine the strength of the individual fibers, it is necessary to disentangle them from the yarn without introducing any damage. Three aramid-based copolymer fibers were selected for the study. The fibers were washed with acetone followed by methanol to remove an organic coating that held the individual fibers in each yarn bundle together. This coating makes it difficult to separate single fibers from the yarn bundle for mechanical testing without damaging the fibers and affecting their strength. After washing, fourier transform infrared (FTIR) spectroscopy was performed on both washed and unwashed samples and the results were compared. This experiment has shown that there are no significant variations in the spectra of poly(p-phenylene-benzimidazole-terephthalamide-co-p-phenylene terephthalamide) (PBIA-co-PPTA1) and PBIA-co-PPTA3 after washing, and only a small variation in intensity for PBIA. This indicates that the acetone and methanol rinses are not adversely affecting the fibers and causing chemical degradation. Additionally, single fiber tensile testing was performed on the washed fibers to characterize their initial tensile strength and strain to failure, and compare those to other reported values. Iterative procedural development was necessary to find a successful method for performing tensile testing on these fibers.

The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation.

Entwirren hohe Festigkeit-Copolymer-Aramid-Fasern um die Bestimmung der mechanischen Eigenschaften ermöglichen

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

Oberflächeneigenschaften von synthetisierten nanoporöse Carbon und Silica-Matrizen

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Extraction of Lignin with High &#946;-O-4 Content by Mild Ethanol Extraction and Its Effect on the Depolymerization Yield

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the emerging elegant procedures to obtain specific aromatic products rely on the lignin substrate having a high content of the readily cleavable &#946;-O-4 linkage as present in the native lignin structure. This provides a miss-match with typical technical lignins that are highly degraded and therefore are low in &#946;-O-4 linkages. Therefore, the extraction yields, and the quality of the obtained lignin are of utmost importance to access new lignin valorization pathways. In this manuscript, a simple protocol is presented to obtain lignins with high &#946;-O-4 content by relatively mild ethanol extraction that can be applied to different lignocellulose sources. Furthermore, analysis procedures to determine the quality of the lignins are presented together with a depolymerization protocol that yields specific phenolic 2-arylmethyl-1,3-dioxolanes, which can be used to evaluate the obtained lignins. The presented results demonstrate the link between lignin quality and potential for the lignins to be depolymerized into specific monomeric aromatic chemicals. Overall, the extraction and depolymerization demonstrates a trade-off between the lignin extraction yield and the retention of the native aryl-ether structure and thus the potential of the lignin to be used as the substrate for the production of chemicals for higher-value applications.

Here, we present a protocol to perform ethanol extraction of lignin from several biomass sources. The effect of the extraction conditions on the lignin yield and &#946;-O-4 content are presented. Selective depolymerization is performed on the obtained lignins to obtain high aromatic monomer products.

Gewinnung von Lignin mit hohen Gehalt an β-O-4 durch milde Ethanol Extraktion und seine Wirkung auf die Depolymerisation Ausbeute

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the ...

A Rhodopsin Transport Assay by High-Content Imaging Analysis

Rhodopsin misfolding mutations lead to rod photoreceptor death that is manifested as autosomal dominant retinitis pigmentosa (RP), a progressive blinding disease that lacks effective treatment. We hypothesize that the cytotoxicity of the misfolded rhodopsin mutant can be alleviated by pharmacologically stabilizing the mutant rhodopsin protein. The P23H mutation, among the other Class II rhodopsin mutations, encodes a structurally unstable rhodopsin mutant protein that is accumulated in the endoplasmic reticulum (ER), whereas the wild type rhodopsin is transported to the plasma membrane in mammalian cells. We previously performed a luminescence-based high-throughput screen (HTS) and identified a group of pharmacological chaperones that rescued the transport of the P23H rhodopsin from ER to the plasma membrane. Here, using an immunostaining method followed by a high-content imaging analysis, we quantified the mutant rhodopsin protein amount in the whole cell and on the plasma membrane. This method is informative and effective to identify true hits from false positives following HTS. Additionally, the high-content image analysis enabled us to quantify multiple parameters from a single experiment to evaluate the pharmacological properties of each compound. Using this assay, we analyzed the effect of 11 different compounds towards six RP associated rhodopsin mutants, obtaining a 2-D pharmacological profile for a quantitative and qualitative understanding about the structural stability of these rhodopsin mutants and efficacy of different compounds towards these mutants.

Here, we described a high-content imaging method to quantify the transport of rhodopsin mutants associated with retinitis pigmentosa. A multiple-wavelength scoring analysis was used to quantify rhodopsin protein on the cell surface or in the whole cell.

Ein Rhodopsin Transport Test von High-Content Imaging-Analyse

Rhodopsin misfolding mutations lead to rod photoreceptor death that is manifested as autosomal dominant retinitis pigmentosa (RP), a progressive blinding ...