このホワイトペーパーで説明する作業は、CII-HK /ポリUイノベーション基金からの助成金によってサポートされていました。さらにサポートが深センピーコックプラン（KQTD2015071616442225）と中国政府の「千タレント」プログラム（Y62HB31601）によって提供されました。また、応用生物学科＆化学技術香港理工大学の持続可能な都市開発のための香港理工大学研究所（RISUD）からのヘルプは大歓迎です。

1 HGMの前処理<ol><li>無水アルコール200mLで500mLのビーカーにHGMを置きます。切れ目のないHGMの低密度は、それがアルコールに懸濁させ、しかし壊れHGMの密度は、アルコールよりも大きいので、それは溶液中に沈殿します。 30分後、さらにアプリケーションのオーブン中で80℃で清潔なスプーン、乾燥を使用して懸濁HGMを収集します。 </li></ol> MCHGMの2合成<ol><li>切れ目のないHGM 5gを、エタノールの47.5 mLの、三口フラスコ内の脱イオン水2.5ミリリットルを置き。 20分（予備混合）400 R /分で混合モーターを使用して攪拌します。 </li><li> TBTを15g、PFOTESを1g、及び200mLのビーカー中の無水アルコール30mLを混合します。定圧漏斗に混合物を注ぎます。 </li><li>三口フラスコの穴の一つに定圧漏斗を挿入します。の速度で三口フラスコに定圧漏斗中に含まれる混合物をドロップ定圧漏斗のバルブを調整することによって達成される7秒ごとに1滴、。 3時間反応を継続します。 </li><li>熱水反応器に三口フラスコからの混合物を注ぎます。 6時間180℃のオーブン中で適切な鋼スリーブに封入された反応器に入れました。 注：反応器は、適切なカバーを持っていることを確認します。それが覆われた後、鋼製のスリーブに原子炉を置きます。スリーブは、カバーで密封されなければなりません。 </li><li>反応が終わった後、大スプーンを使用して熱水反応器中に懸濁したサンプルを集めます。 MCHGMを得るために4時間80℃でサンプルを乾燥させます。 </li></ol> F-SCHGM 3.合成<ol><li>切れ目のないHGM 5gを、無水エタノール47.5 mLを、三口フラスコに脱イオン水2.5 mLを加え。 20分（予備混合）400 R /分で混合モーターを使用して攪拌します。 200mLのビーカーにPFOTES 1g及び無水エタノール30mlを混合します。 PFOTESと絶対的な電子転送定圧漏斗にthanol混合物。 </li><li>三口フラスコに定圧漏斗を挿入します。 7秒ごとに1滴の速度で三口フラスコに定圧漏斗中に含まれる混合物を落とします。反応を3時間実行してみましょう。 </li><li>熱水反応器に三つ口フラスコからの混合物を移します。 6時間180℃のオーブン内に密封反応器に入れました。反応が終わった後、大スプーンを使用して熱水反応器中に懸濁したサンプルを集めます。 F-SCHGMを得るために、4時間80℃でサンプルを乾燥させます。 </li></ol> TiをSCHGM 4.合成<ol><li>切れ目のないHGM 5gを、無水エタノール47.5 mLを、三口フラスコ内の脱イオン水2.5ミリリットルを置き。 20分（予備混合）400 R /分で撹拌しました。 TBT 15gの 200ミリリットルのビーカーに無水エタノール30mlを混合します。定圧漏斗にTBTと無水エタノールの混合物を移します。 </li><li>定PRESを挿入必ず三つ口フラスコに注ぎ込みます。 7秒ごとに1滴の速度で三口フラスコに定圧漏斗に混合物を落とします。反応を3時間実行してみましょう。 </li><li>熱水反応器に三つ口フラスコからの混合物を移します。 6時間180℃のオーブン内に密封反応器に入れました。反応が終わった後の熱水反応器のサンプルを収集します。 TiをSCHGMを得るために、4時間80℃でサンプルを乾燥させます。 </li></ol> 5.特徴付け<ol><li>すべてのサンプルのXRD特徴付けを行っています。 CuのKα線（λ= 0.15406 nm）を10℃から80℃の範囲の2θで汎用性の高い、多目的X線回折装置を使用してデータを収集します。 </li><li>走査型電子顕微鏡20、金サンプルを噴霧後21枚の画像を取得します。 SEMの試験中、EDSは、特定の領域にある行っています。 </li><li>計測接触角 接触角ゴニオメーター22を使用して、水滴の体積は10μLでなければなりません。 </li><li>表面の傾斜角度を変更することにより、滑り角度23を測定します。水滴がちょうど下にスライドできるようになるまでの角度を最小限に抑えます。 <ol><li> （26ミリメートル×76ミリメートルX 2ミリメートルサイズ）のガラスシート上に両面テープを貼り。スプーンを使用して、均一にテープ上の粉末（F-SCHGM又はMCHGM）を置きます。注射器を使用して、水滴（容量：0.05 ml）を追加し、粉末表面に。 </li><li>接触角ゴニオメータのモータプラットフォーム上にガラス板を置きます。 1°/秒の速度でモータプラットフォームを傾いてガラスシートを傾け。水滴がスライドし始めたときにモータを停止。チルト角は転落角です。 </li></ol></li><li>分光光度計24を使用して反射率スペクトルを測定します。注：波長を450nmから2550 nmのです。 </li><li>全てのサンプルの熱伝導率を測定します熱伝導率計25を使用して。 </li></ol>

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The authors have nothing to disclose.

本稿では、プロトコルにおける重要なステップは、水熱法です。これは、TiO 2、最終反射率、及び超疎水性の形成に影響を与えます。温度制御及び反応時間も非常に重要です。反応条件が変更された場合、最終製品が不備ことができます。 この方法は、一の段階で超疎水性の高いIR反射HGMを合成する簡単な方法を提供します。以前の研究では、超疎水性及び反射?...

中空ガラス微小球（HGM）が10〜100μmのサイズ範囲の無機材料です。それらは、優れた分散、高い流動性、低密度、優れた断熱性1、2、3、4のような多くの有用な機能を実証します。なぜなら、その中空構造の、HGMは非常に低い熱伝導率10、11を有しています。これらの理由から、それらは航空宇宙等工学5、深海探査6、7、水素貯蔵8、9、しかし、彼らはまだ、このような低強度などのいくつかの欠点を実証するなど、多くの分野で適用されています。また、IR光は、HGMを透過して背後に被写体を加熱することが可能です。そのためE、HGMに表面修飾は、放射熱伝達を減少させるために不可欠です。効果的な方法は、HGM表面上にコーティングするためにIR遮断材料です。半導体として、TiO 2は 、このような光触媒12、13、太陽電池の開発、センサーの製造14、環境アプリケーション15、およびエネルギー貯蔵16などの多くの分野で使用されてきました。加えて、それはまた、可視光と赤外バンド17、18、19の低い放射率を示しています。したがって、我々の目的のために、TiO 2は 、比較的低価格で高性能のために賢明な選択でした。 しかし、コーティングは真剣TiOの反射率に影響を与える、汚染物質が汚染するのは非常に簡単です。反射率は徐々に減らす必要があります。したがって、SELF-クリーニングコーティングは、汚れからコーティングを防ぐために、そのようなコーティングの作業時間を延長することが不可欠です。 本稿では、ソフト化学法は、超疎水性のTiO 2被覆HGM開発するために使用しました。テトラブチルチタネート（TBT）及び1H、1H、2H、2H- perfluorooctyltriethoxysilane（PFOTES）は、それぞれ、Ti原料及び超疎水性剤として選択しました。彼らは、加水分解し、HGM表面上に堆積させました。その後、熱水処理後、アナターゼTiO 2が HGMの表面上に形成され、超疎水特性が残りました。比較のために、単一の被覆HGM（F-SCHGM）及びTiO 2の単一被覆HGMチタン（Ti-SCHGM）PFOTES同様に合成しました。合成スキームを図1に示されています。

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			<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

この原稿は、超疎水性の高いIR反射中空ガラス微小球（HGM）を開発するためのソフト化学法を提案します。アナターゼ型のTiO 2と超疎水性剤が一の工程でHGM表面上に塗布しました。 TBTとPFOTESは、それぞれ、Ti原料及び超疎水性剤として選択しました。彼らは、両方のHGMに塗布し、熱水処理後、TBTは、TiO 2をアナターゼになりました。このように、PFOTES / TiO 2は HGM（MCHGM）を調製したコーティングされました。比較のために、単一の被覆HGM（F-SCHGM）及びTiO 2の単一被覆HGMチタン（Ti-SCHGM）PFOTES同様に合成しました。 HGM表面上PFOTESとTiO 2つのコーティングは、X線回折（XRD）、走査電子顕微鏡（SEM）及びエネルギー分散型検出器（EDS）の特徴付けを介して実証されました。 MCHGMは141.2の接触角を有する、より高い接触角（153°）が、F-SCHGMより低い転落角（16°）を示しました6;そして、67°の角度をスライドさせます。加えて、両方のTi-SCHGMとMCHGM元のHGMとF-SCHGMよりも約5.8％高かった同様のIR反射率値を、表示しました。また、PFOTESコーティングはほとんど熱伝導率を変えました。したがって、F-SCHGMは、0.0479 W /（M・K）の熱伝導率と、かなり0.0475 W /（M・K）であった元のHGM、のようでした。 MCHGMとTi-SCHGMも同様でした。それらの熱伝導率の値は、それぞれ、0.0543 W /（M・K）及び0.0543 W /（M・K）でした。 TiO 2のコーティングは、わずかに熱伝導率を増加したが、反射率の増加に伴って、全体的な断熱性が向上しました。 IR反射性をHGMコーティングによって提供されるので、コーティングが汚れている場合、最終的に、反射率が低下します。したがって、超疎水性コーティングと、表面が汚染から保護され、その寿命も長くなります。

ステップ4.4におけるテストサンプルの多くの特徴および特性を明らかにする。 XRD（ 図2）がアナターゼTiOの形成を反映しています。 SEM（ 図3）及びEDS（ 図4）HGM表面上にコーティングされたTiO 2とPFOTESを表示します。接触角（ 図5）および転落角（ 図6）のテストが超疎水性を表します。可...

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.

たTiO<sub&gt; 2</subソフト化学法により合成超疎水性と高IR反射特性を持つ&gt;でコーティングされた中空ガラスマイクロスフェア

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 ビュー.  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.

ビデオ: 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.

ビスiminoguanidiniumリガンドと選択的結晶化により硫酸の分離

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

化学

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.

強化された電子導電特性を持つFeドープアルミノシリケートナノチューブの合成とキャラクタリゼーション

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.

高圧液体クロマトグラフィー（HPLC）とグルコシノレートの抽出および分析のための簡単な方法

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.

抽出と神経伝達物質カテコールアミン及びその代謝物の高速液体クロマトグラフィーによる分析のための便利な方法

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.

中空のポリスチレン粒子と炭化水素とフッ素オイルから成るヤヌス液滴のラジカル重合によるマイクロ カプセルの調製

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.

Nb2O5の合成化学沈殿法変更高表面積一括ニッケル触媒

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.

その力学的特性の測定を可能にする高強度共重合体のアラミド繊維を disentangling

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.

合成多孔性カーボンとシリカ マトリックスの表面特性

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.

高 β-O-4 コンテンツによるリグニンの抽出軽度エタノール抽出と脱重合の収量に及ぼす影響

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.

高コンテンツ イメージング解析によるロドプシン輸送アッセイ

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