当社は、電気化学的な実験や計測機器（LSCとJTH）のサポートのための化学のバージニア軍事研究所（VMI）部門を認める。学部長のVMI事務所はJoveの出版物に関連した制作費をサポートしていました。私たちは、UNC EFRCを認める：化合物合成や材料特性評価のサポートのためのソーラー燃料のためのセンター、エネルギーフロンティア研究センター、米国エネルギー省によって資金を供給、科学局、賞番号DE-SC0001011下の基礎エネルギー科学のオフィス、（DPH ）。

1.論理合成1 によると- ：合成1（図4; 5,5&#39;- dvbpyは5,5&#39;-ジビニル-2,2&#39;-ビピリジンであるターピリジン、2 &#39;&#39; PhTpyは4&#39;-フェニル-2,2である「6」）プロシージャは、以前に説明した。18 2.電解液中の1の1.3 mMのモノマー溶液を準備<ol><li> 、アセトニトリル中で、TBAPF 6、MeCN中のテトラn個 -butylammonium六フッ化リン酸の0.1 M株式電解質溶液を準備します。 <ol><li>外来のH 2 Oを除去するために24時間、活性化した3Åモレキュラーシーブ、またはK 2 CO 3上のMeCNを置き</li><li>メスフラスコを乾燥さ25.00ミリリットル炎にTBAPF 6（0.969グラム、2.50ミリモル）を配置します。 </li><li>乾燥したMeCN中から、分子ふるいまたはK 2 CO 3微粒子を濾過し、25.00ミリリットルのTBAPFを含むメスフラスコをもたらす<sub&gt;の6のボリュームに。 </li></ol></li><li> 4ドラムのバイアルまたは10ミリリットル丸底フラスコに、乾燥1（0.0049グラム、5.2×10 -6モル）を配置し、MeCN中0.1MのTBAPF 6の原液の4.00ミリリットルを追加します。 </li><li>中多孔性ガラスフリットで区切られた各区画と、3室セルの中央区画に1の赤橙色着色された電解液の3.5〜4.0ミリリットルを転送します。 </li><li>すぐに外区画への漏洩を防止するMeCN中の残りの乾燥0.1 M TBAPF 6の一部と、中心区画原液として同じ高さに3室セルの外側の区画を満たす。注：異なる区画内の溶液がゆっくりと混ぜて、溶媒の高さが同じでない場合、大幅にメインコンパートメントの濃度が変化しますので、時間が重要な要因である。 </li></ol>直径3mmのガラス3. Electropolymerize 1Yカーボン電極または1.0センチメートル2 FTO電極<ol><li>窒素/アルゴンガス抜き管用及び電極用セプタムを準備します。 <ol><li> 3ゴム隔膜のそれぞれにスリットをカットし、スリットを介して薄いポリテトラフルオロエチレン、PTFE、チューブをガイド。 </li><li> 、セプタムのいずれかを使用してのAg / AgNO 3を参照電極をスライドさせ、外側区画のいずれかの参照電極/ PTFEチューブ/隔壁を配置し、セプタムでコンパートメントを密閉する ​​。 </li><li>異なるセプタム場所を通して外側の区画のいずれかで白金線/ PTFEチューブ/セプタムを白金線/ガーゼ対極ガイド、およびセプタムでコンパートメントをシール。スリットは、ワイヤを曲げ防止するのに十分な剛性を十分に大きなまたはワイヤでない場合には、隔壁を通して白金線対電極をガイドするために大口径の針を使用する。 </li><li>残りのセプタムを通して新鮮に洗練された3ミリメートルグラッシーカーボン電極を導き、それはそのような電極がsuspeであることを置く溶液中のndedまたは、FTOスライド用、ワニ口クリップFTOスライドをクランプし、水没時のスライドの導電側は対極に垂直であることを確認して、その後、隔壁を通してワニ口クリップに接続されたワイヤをガイド。 <ol><li>ポーランドに - 、その後、濡れた研磨パッド上にアルミナ（0.5μm）を配置することでガラス状炭素を研磨パッドに垂直に電極を保持した状態で30秒間8の字運動に電極を移動：グラッシーカーボン電極を挿入する前に電極のすべての側面に均等に-し、MeCN噴出ボトルリンスに続いて、H 2 O水の噴出ボトルに残っているアルミナを洗い流してください。 </li><li> FTOスライドクランプする前に：スライドの10×10 mmの部分が露出するように30×10 mmのFTOスライドの中央部分の周りの非導電性カプトンテープの複数の層を包む。 </li><li> POSITでFTOスライドを保持/配置することによって、FTOスライドの紫外可視スペクトルを収集一貫性を確保するために、予め定められた分光計のビーム経路におけるイオン。 </li></ol></li></ol></li><li> 3コンパートメント電気化学セル内の溶液を脱気。 <ol><li>窒素/アルゴン供給にタイゴンチューブの一端を接続し、MeCNを含むガス洗浄機にもう一方の端を接続します。 </li><li>窒素/アルゴン洗浄し流出をMeCNに一端を接続し、タイゴンチューブの別の部分をカットし、4ウェイスプリッタにもう一方の端を接続します。 </li><li> 4ウェイスプリッタの3残りの接続にPTFEチューブを接続します。 </li><li>各区画にソリューションにPTFEチューブを浸し、溶液の急速な泡立ちが始まるように窒素/アルゴンの流量をオンにしてください。 </li><li>システム上の不活性ガスの正圧を維持するために、この溶液を防止するために、上の窒素/アルゴンの流量を残して、単に溶液の表面の上にPTFEチューブを引っ張り、その後、5~10分間この溶液を脱曝気続ける℃バブリングによって引き起こさonvection。 </li></ol></li><li>電気化学的な実験を行う。 <ol><li> 3室セル内の適切な電極にポテンショスタットから電極を接続します。 </li><li>サイクリックボルタンメトリーを行って、CV、次のパラメータを使用して実験：スイッチング電位= 0 Vと-1.81 V。スキャン/掃引速度= 100 mVの/秒。サイクル= 5の数。 </li><li> CV実験が完了すると、重合溶液から加工（グラッシーカーボンまたはFTO）電極を除去し、穏やかに残りのモノマー溶液を除去するために、ピペットまたは噴霧ボトルからMeCNで電極の表面をすすぐ。 </li></ol></li></ol> 4.表面被覆率の決定<ol><li>対極及び参照電極（electropolymerizatioで使用、好ましくは同じ基準電極を含む電気化学セルで0.1 M TBAPF 6 / MeCN中の新たに調製した溶液でリンス作用電極を配置n）である。 </li><li>サイクリックボルタンメトリーを行って、CV、次のパラメータを使用して実験：スイッチング電位= 0と1.5 V。スキャン/掃引速度= 100 mVの/秒。サイクル数= 15。 </li><li> 、吸着したelectropolymerのRu（III / II）カップルのための陽極と陰極のピーク下電荷を統合し、陽極と陰極のピーク下の電荷を平均化し、式（1）は、表面被覆率を決定する使用。 </li><li> FTOスライドの場合：場所/ビーム経路は着色フィルムを通過するように、UV-Visのサンプルホルダの前方の所定位置におけるFTOスライドを保持する。 FTOスライドを湿式または乾式であるが、ブランクスペクトル下で収集したのと同じ条件下で比較することができる。 </li><li>フィルム自体の吸収スペクトルを生成するために、フィルム·オン·FTOのスペクトルから電解重合する前に、その特定のスライド用に収集したFTOスペクトルを得られたスペクトルを差し引く。 </li></ol>

<ol>
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M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+and+Spectroelectrochemical+Investigations+into+the+Nature+of+Charge-Trapping+in+Electrochemically-Generated+Homopolymer+Films+of+Tris(4-vinyl-4&#8216;-methyl-2,2&#8216;-bipyridine)ruthenium(II).">Electrochemical and Spectroelectrochemical Investigations into the Nature of Charge-Trapping in Electrochemically-Generated Homopolymer Films of Tris(4-vinyl-4&#8216;-methyl-2,2&#8216;-bipyridine)ruthenium(II).</a> The Journal of Physical Chemistry B. 105, 8718-8724 (2001).</li><li>Laviron, E., Roullier, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+for+a+surface+redox+reaction+with+interactions+between+the+adsorbed+molecules:+Applications+to+modified+electrodes.">General expression of the linear potential sweep voltammogram for a surface redox reaction with interactions between the adsorbed molecules: Applications to modified electrodes.</a> J. Electroanal. Chem. Interfacial Electrochem. 115, 65-74 (1980).</li><li>Laviron, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+in+the+case+of+diffusionless+electrochemical+systems.">General expression of the linear potential sweep voltammogram in the case of diffusionless electrochemical systems.</a> J. Electroanal. Chem. 101, 19-28 (1979).</li><li>Ratcliff, E. L., Jenkins, J. L., Nebesny, K., Armstrong, N. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposited,+&#34;Textured&#34;+Poly(3-hexyl-thiophene)+(e-P3HT)+Films+for+Photovoltaic+Applications.">Electrodeposited, &#34;Textured&#34; Poly(3-hexyl-thiophene) (e-P3HT) Films for Photovoltaic Applications.</a> Chemistry of Materials. 20, 5796-5806 (2008).</li></ol>

No conflicts of interest declared.

電解重合は、他の技術に共通していない制御可能な変数の大規模な範囲を提供しています。試薬（モノマー）の濃度、温度、溶媒等のような標準的な反応変数に加えて、電解重合は、さらに、電気化学的方法に共通の電気化学実験パラメータによって制御することができる。 CVは、電位を切り替え、スキャン速度、およびサイクル数はelectropolymersの堆積に影響を与える。例えば、リガ?...

電解重合を直接電極の表面でモノマー前駆体の重合を開始するために印加電位を利用して、薄い電気および/ ​​または電極と半導体表面に光化学的に活性なポリピリフィルムを製造するために利用された重合法である。1-4電気触媒、 5-10電子移動、11、12光化学、13-16エレクトロ17と協調化学18は 、電解膜で研究されてきた。この技術は、第一ビニール3、5、7、8、11-15、19、20、およびピロール6,9の電解重合のためのマイヤー·マレーのコラボレーションでノースカロライナ大学で開発された、21〜24は私を誘導体化導電性基板の上に、様々タル複合体。 図1 electropolymersを生成した金属錯体に配位した場合に、共通のベースピリジル配位子の数を示す。ピロール官能化リガンドと、電解が（ 図2）、酸化電解重合で得られた、ピロール部分の酸化によって開始される一方、還元電解重合では、ビニル基含有化合物の電解重合は、ビニル基にコンジュゲートピリジル配位子の還元時に発生する。電解技術が直接電極に実質的に任意の遷移金属錯体を取り付けるための一般化された方法を提供することを目的として開発された。メソッドの汎用性はelectropolymer修正された電極の数々の調査への扉を開きます。 電極への直接結合を含む他の取り付けストラテジーとは対照的に、電解重合は前売りを提供電極表面の事前修正を必要としないアンテージ。したがって、それは関係なく、表面組成または形態の、導電性基板は任意の数に適用することができる4、10、25、26、この汎用性は、長さが成長するポリマーの物性を変化させることの結果である。モノマーは、電解液中に可溶性であるが、重合がrigidifiesを発生し、架橋フィルムとして、沈殿および物理吸着電極表面（ 図3）が発生する。27 一般に太陽燃料研究に使用される高められたpHは、で不安定であり、酸化物の水中での表面、又はホスホネート誘導体化錯体に不安定であり、酸化物表面に結合したカルボキシレートと比較して、これらの界面電極高分子フィルム構造体は、安定性の追加の利点を提供する大pH範囲（0〜14）を介して、有機溶媒と水を含む様々なメディアで。28-30カルボキシレートまたはホスホネート誘導体化複合体·インタフェース構造が単層表面被覆率に制限されているのに対し、電解重合はまた、サブモノレイヤーから同等物単層の数十または数百に、見かけの表面被覆率の大範囲が膜を堆積することができます。 、ピリジルおよびポリピリジル化合物を含有するビニルピロール、任意の数の重合が可能であるもののの[Ru II（PhTpy）（5,5&#39;- dvbpy）（MeCN中）]（PF 6）2、（1; PhTpy 4&#39;-フェニルである-2,2 &#39;：6&#39;、2 &#39;&#39; -ターピリジン; 5,5&#39;- dvbpyは5,5&#39;-ジビニル-2,2&#39;-ビピリジンであり; 図4）は 、還元電解重合を実証するためのモデルの複合体として利用されるガラス状炭素とフッ素ドープ酸化スズで、FTO、本報告書内の電極1は 、その金属-李に、潜在的な電極触媒の用途を有する近代的electropolymer前駆体の例であり、GAND電荷移動、MLCT、光スペクトルの可視領域内にある吸収スペクトルは、紫外可視分光法を用いて調査することができます。18、30 1のためにここに提示され、いくつかの結果は、すでにわずかに変更された形で公開されていることに注意してください。18

<table border="0" cellpadding="0" cellspacing="0" width="652">
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		<tr height="21">
			<td height="21" style="height:21px;width:384px;">Name of Reagent/ Equipment</td>
			<td style="width:108px;">Company</td>
			<td style="width:160px;">Catalog Number</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Tetrabutylammonium hexafluorophosphate for electrochemical analysis, &#8805;99.0%,&#160;</td>
			<td>Sigma-Aldrich</td>
			<td>86879-25G</td>
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			<td height="20" style="height:20px;width:384px;">Acetonitrile&#160;(Optima LC/MS), Fisher Chemical</td>
			<td>Fisher Scientific</td>
			<td>A955-4</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">3 mm dia. Glassy Carbon Working Electrode</td>
			<td>CH Instruments</td>
			<td>CH104</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Non-Aqueous Ag/Ag+ Reference Electrode w/ porous Teflon Tip</td>
			<td>CH Instruments</td>
			<td>CHI112</td>
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			<td height="20" style="height:20px;">Platinum&#160;gauze</td>
			<td>Alfa Aesar</td>
			<td>AA10282FF&#160;</td>
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			<td height="20" style="height:20px;">Electrode Polishing Kit</td>
			<td>CH Instruments</td>
			<td>CHI120</td>
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			<td height="20" style="height:20px;width:384px;">Cole-Parmer KAPTON TAPE&#160;1/2IN X 36 YD</td>
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			<td height="20" style="height:20px;width:384px;">Fisherbrand Polypropylene Tubing&#160;4-Way&#160;Connectors</td>
			<td>Fisher Scientific</td>
			<td>15-315-32B</td>
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			<td height="20" style="height:20px;">500mL Bottle, Gas Washing, Tall Form, Coarse Frit</td>
			<td>Chemglass</td>
			<td>CG-1114-15</td>
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		<tr height="20">
			<td height="20" style="height:20px;">3 compartment H-Cell for electrochemistry</td>
			<td colspan="2">Custom made H-cell with 3 compartments</td>
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	</tbody>
</table>

reductive electropolymerization of a vinyl-containing poly-pyridyl complex on glassy carbon and fluorine-doped tin oxide electrodes

制御可能な電極表面の修飾は、フィールド、太陽燃料アプリケーションで特に数が重要である。電解重合は、ヘルムホルツ層における基質の重合を開始するために印加電位を利用することにより、電極の表面に高分子フィルムを電着物つの表面改質技術である。この有用な技術は、最初に1980年代初期にノースカロライナ大学チャペルヒル校で、マレー·マイヤーのコラボレーションによって確立され、単量体の基板などの無機複合体を含有するフィルムの多数の物理現象を研究するために利用された。ここでは、ガラス状炭素、フッ素ドープ酸化スズコーティングされた電極上にビニル含有ポリピリジル錯体の還元電解重合を行うことにより、無機複合体被覆電極のための手順を強調する。電気化学セル構成およびトラブルシューティングの手順上の勧告が含まれています。メールではないがxplicitlyここで説明し、ピロール含有化合物の酸化電解重合は、ビニル系還元電解と同様の手順に従うが、はるかに感度が低い酸素および水にある。

所定のCV実験（プロトコルテキストSTEP 3.3.2）の進行状況を観察したときElectropolymer成長が最も容易に認識されている。 図5は1と0.071センチメートル2（3ミリメートル直径）グラッシーカーボン電極上にelectropolymer成長を例示している。実験の最初のサイクルはますます強化された電流であり、 第 1および第 2 のリガンドを中心削減の波を通じて、ほ?...

Watch this Scientific Journal Video about Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes at JoVE.com

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

グラッシーカーボンとフ​​ッ素ドープ酸化スズ電極上にビニル含有ポリピリジル錯体の還元電解重合

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

reductive-electropolymerization-vinyl-containing-poly-pyridyl-complex

Research

JoVE Journal

Chemistry

11.7K ビュー.  Virginia Military Institute. A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization. 

ビデオ: Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Improved In-gel Reductive &#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of biological samples. Similar approaches, that would allow in-depth analysis of the glycans carried by glycoproteins resolved by SDS-PAGE, require special considerations in order to maximize recovery and sensitivity when using mass spectrometry (MS) as the detection method. A major hurdle to be overcome in achieving high-quality data is the removal of gel-derived contaminants that interfere with MS analysis. The sample workflow presented here is robust, efficient, and eliminates the need for in-line HPLC clean-up prior to MS. Gel pieces containing target proteins are washed in acetonitrile, water, and ethyl acetate to remove contaminants, including polymeric acrylamide fragments. O-linked glycans are released from target proteins by in-gel reductive &#946;-elimination and recovered through robust, simple clean-up procedures. An advantage of this workflow is that it improves sensitivity for detecting and characterizing sulfated glycans. These procedures produce an efficient separation of sulfated permethylated glycans from non-sulfated (sialylated and neutral) permethylated glycans by a rapid phase-partition prior to MS analysis, and thereby enhance glycomic and sulfoglycomic analyses of glycoproteins resolved by SDS-PAGE.

Improved In-gel Reductive &amp;#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

In order to comprehensively explore the diversity of O-linked glycans, a new procedure for in-gel reductive &#946;-elimination, combined with permethylation and a rapid phase-partition method, is applied to the analysis of O-linked glycans directly released from glycoproteins resolved by SDS-PAGE and amenable to subsequent glycomic analysis by mass spectrometry.

質量分析法による総合的なO-結合およびスルホグライコミクスのための改良されたゲル内還元β脱離

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of ...

化学

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

土壌カラムを通して表面修飾カーボンナノチューブの輸送

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

CdSeの@のCdSナノロッド上にイリジウム酸化物ナノ粒子の光化学酸化成長

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

オンライン複雑な炭化水素マトリックス中の窒素含有化合物の分析

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Investigations on the Ga(III) Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) complex and protocols for the preparation of its novel non-radioactive, i.e., natural Ga(III) as well as radioactive 68Ga complex. The ligand as well as the Ga(III) complex were characterized by nuclear magnetic resonance (NMR) spectroscopy, mass spectrometry and elemental analysis. 68Ga was obtained by a standard elution method from a 68Ge/68Ga generator. Experiments to evaluate the 68Ga-labeling efficiency of EOB-DTPA at pH 3.8&#8211;4.0 were performed. Established analysis techniques radio TLC (thin layer chromatography) and radio HPLC (high performance liquid chromatography) were used to determine the radiochemical purity of the tracer. As a first investigation of the 68Ga tracers&#39; lipophilicity the n-octanol/water distribution coefficient of 68Ga species present in a pH 7.4 solution was determined by an extraction method. In vitro stability measurements of the tracer in various media at physiological pH were performed, revealing different rates of decomposition.

Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

A procedure for the isolation of EOB-DTPA and subsequent complexation with natural Ga(III) and 68Ga is presented herein, as well as a thorough analysis of all compounds and investigations on labeling efficiency, in vitro stability and the n-octanol/water distribution coefficient of the radiolabeled complex.

EOB-DTPAとそのののGa（III）錯体に関する研究<sup&gt; 68</sup&gt; Gaの放射性標識アナログ

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

ポリスチレン自己組織を有効にして異方的不均一性と多層カーボンナノ チューブを移植

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

電気化学インピー ダンス分光電気化学定数推定法のためのツールとして

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

ミル-96、UiO-66-NH2原子層のソルボサーマル合成繊維のマット上金属酸化皮膜に堆積

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Negative Additive Manufacturing of Complex Shaped Boron Carbides

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for high wear, high hardness, and lightweight material applications such as armors. To overcome this challenge, negative additive manufacturing (AM) is employed to produce complex geometries of boron carbides at various length scales. Negative AM first involves gelcasting a suspension into a 3D-printed plastic mold. The mold is then dissolved away, leaving behind a green body as a negative copy. Resorcinol-formaldehyde (RF) is used as a novel gelling agent because unlike traditional hydrogels, there is little to no shrinkage, which allows for extremely complex molds to be used. Furthermore, this gelling agent can be pyrolyzed to leave behind ~50 wt% carbon, which is a highly effective sintering aid for B4C. Due to this highly homogenous distribution of in situ carbon within the B4C matrix, less than 2% porosity can be achieved after sintering. This protocol highlights in detail the methodology for creating near fully dense boron carbide parts with highly complex geometries.

A method called negative additive manufacturing is used to produce near fully dense complex shaped boron carbide parts of various length scales. This technique is possible via the formulation of a novel suspension involving resorcinol-formaldehyde as a unique gelling agent that leaves behind a homogenous carbon sintering aid after pyrolysis.

負の複雑な形をした炭化ホウ素の添加剤の製造

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for ...

グラッシーカーボンとフ​​ッ素ドープ酸化スズ電極上にビニル含有ポリピリジル錯体の還元電解重合

グラッシーカーボンとフッ素ドープ酸化スズ電極上にビニル含有ポリピリジル錯体の還元電解重合