Department of Chemistry

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IIT Hyderabad

The decomposition of trichloroethylene (TCE) by non-thermal plasma was investigated in a dielectric barrier discharge (DBD) reactor with a copper rod inner electrode and compared with a plasma-catalytic reactor. The particularity of the plasma-catalytic reactor is the inner electrode made of sintered metal fibers (SMF) coated by transition metal oxides. In order to optimize the geometry of the plasma reactor, the efficiency of TCE removal was compared for different discharge gap lengths in the range of 1-5 mm. Shorter gap lengths (1-3 mm) appear to be more advantageous with respect to TCE conversion. In this case TCE conversion varies between 67% and 100% for input energy densities in the range of 80-480 J/l, while for the 5 mm discharge gap the conversion was lower (53-97%) for similar values of the input energy. As a result of TCE oxidation carbon monoxide and carbon dioxide were detected in the effluent gas. Their selectivity was rather low, in the range 14-24% for CO2 and 11-23% for CO, and was not influenced by the gap length. Several other chlorinated organic compounds were detected as reaction products. When using MnOx/SMF catalysts as the inner electrode of the DBD reactor, the TCE conversion was significantly enhanced, reaching ∼95% at 150 J/l input energy. The selectivity to CO2 showed a major increase as compared to the case without catalysts, reaching 58% for input energies above 550 J/l. © 2007 Elsevier B.V. All rights reserved.

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Fulltext

Applied Catalysis B: Environmental

Improved performance of non-thermal plasma reactor during decomposition of trichloroethylene: Optimization of the reactor geometry and introduction of catalytic electrode

Abatement of trichloroethylene (TCE, 250 ppm in air) was studied in a novel nonthermal plasma (NTP) dielectric barrier discharge reactor with an inner electrode made of sintered metal fibers (SMF). The SMF electrodes modified with TiO2 and MnO2 were observed to be catalytically active. Their efficiency in TCE decomposition was compared with a Cu inner electrode. The SMF electrode modified with MnO2 and TiO2 catalyst effectively destroys TCE due to the synergy between plasma excitation of the TCE molecules and their catalytic oxidation. The latter process was observed to be further enhanced by photocatalysis since TiO2 absorbs the UV light produced by the NTP. These innovative TiO2-modified SMF electrodes were characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM), confirming formation of titania anatase, whereas the emission spectrum of the plasma showed the presence of ultraviolet light. © 2007 American Chemical Society.

Journal of Physical Chemistry C

Nonthermal plasma abatement of trichloroethylene enhanced by photocatalysis

Tungsten oxide (WO3) thin film mesophases encompassing a well-organized network of grains with a triclinic phase and pores with diameters in the range of 2-5 nm were generated at room temperature by template-assisted electrodeposition involving a novel combination of ionic and polymeric surfactants. Electron microscopy studies revealed the surface texture of the films annealed at 250 and 500 °C to be primarily composed of randomly oriented rod and sheet-like shapes and the bulk structure of these films to ensconce fibril-like shapes and distinct spherical nanoparticles, along with elongated pores. Coloration efficiency, transmission modulation and charge density for lithium insertion are greater, switching rates are faster (colors in 8.8 s and bleaches in 1.5 s for a 50% transmittance change) and cycling stability is superior for the as-deposited film as compared with the annealed WO3 films. The superior electrochromic performance characteristics of the as-deposited WO3 coatings are a direct manifestation of the mesoporosity over multiple length scales, a good lateral organization of grains and pores which facilitate ion insertion and extraction, and a large number of accessible surface sites which ensure a high proportion of W5+ color centers in the film upon lithium intercalation. In spite of the retention of a porous structure by the film annealed at 500 °C, the poor electrochromic response of the annealed films is attributed to the coarse grain rod-, sheet- and fiber-like framework, which efficiently obstructs lithium ion movement and uptake. © 2007 Acta Materialia Inc.

Acta Materialia

Electro-optical response of tungsten oxide thin film nanostructures processed by a template-assisted electrodeposition route

TiO2 nanostructures of particles and wires have been processed by employing a sol-gel technique and subsequent suitable annealing treatments. A systematic evaluation of phase transformations and morphological features has been investigated exploiting the electron beam imaging and corresponding reciprocal space interpretations. © 2007 IEEE.

Proceedings of the 14th International Workshop on the Physics of Semiconductor Devices, IWPSD

Microstructural development and phase transformations in TiO2 nanostructures

The first enantiospecific total synthesis of the tricyclic sesquiterpene (+)-seychellene, starting from (R)-carvone via (S)-3-methylcarvone, has been accomplished employing a combination of an intermolecular Michael addition-intramolecular Michael addition sequence and an intramolecular alkylation reaction for the generation of the two vicinal quaternary carbon atoms. © 2006 Elsevier Ltd. All rights reserved.

Tetrahedron Letters

The first enantiospecific total synthesis of (+)-seychellene

An efficient approach to the aromatic sesquiterpene cuparene has been described starting from the readily available β-ionone and employing a combination of epoxide rearrangement-based ring-contraction and ring-closing metathesis reactions as key steps. Copyright © Taylor & Francis Group, LLC.

Synthetic Communications

RCM-based approach to (±)-cuparene

In the title compound, (C11H21N2)[Er(C8H8)2], the anion displays the sandwich form with planar and parallel cyclo-octa-tetra-enyl ligands. The perpendicular distances of the Er atom from the C8 planes are 1.8809 (7) and 1.8476 (8) Å, with individual Er - C bond lengths in the range 2.596 (2)-2.651 (2) Å. The extended structure consists of chains of alternating anions and cations parallel to (101); residues are connected by C - H⋯π inter-actions and neighbouring formula units are related by an n glide plane. © International Union of Crystallography 2007.

Acta Crystallographica Section E: Structure Reports Online

1,3-Diisopropylimidazolium bis-(cyclo-octatetraenyl)erbate(III)

Nitrosylruthenium derivatives having NO+ and NO. states have been synthesized in a stepwise manner starting from [Ru II(trpy)(pdt)(Cl)](ClO4) {[1](ClO4)} → [RuII(trpy)(pdt)-(CH3CN)](ClO4)2 {[2](ClO4)2] → [RuII(trpy)(pdt)(NO 2)](C1O4) ([3](ClO4)} → [Ru II(trpy)(pdt)(NO+)](ClO4)3 {[4](ClO4)3} → [RuII(trpy)(pdt)(NO .)](CLO4)2 {[4](ClO4)2} [trpy = 2,2′:6′,2″-terpyridine, pdt = 5,6-diphenyl-3-pyridyl- as-triazine]. The molecular identity of [1](ClO4) and [2](ClO 4)2 and the subsequent stereoretentive transformation of [1](ClO4) → [2]-(ClO4)2 have been authenticated by single-crystal X-ray structures. Electrochemical and spectral features are investigated as a function of the monodentate ligands (Cl -, CH3CN, NO2-, NO+, NO.). The kinetic and thermodynamic aspects of the reaction of the moderately strong electrophilic {RuII-NO+} center [ν(NO): 1944 cm-1] in [4]3+ with a nucleophile such as OH- have been studied. The nitrosyl species [RuII(trpy) (pdt)-(NO+)]3+ ([4]3+) can be selectively reduced to [RuII(trpy)(pdt)-(NO.)]2+ ([4] 2+) electrochemically as well as chemically by hydrazine hydrate. On exposure to light an acetonitrile solution of [RuII(trpy)(pdt) (NO.)]2+ ([4]2+) undergoes slow photocleavage of the RuII-NO bond over a period of 4 h, resulting in the corresponding solvated species [RuII(trpy)(pdt)(CH 3CN)]2+ ([2]2+). The rate of photolability of the RuII-NO bond in [4]2+ has been monitored spectrophotometrically. © Wiley-VCH Verlag GmbH &amp; Co. KGaA, 2007.

European Journal of Inorganic Chemistry

Synthesis and spectro-electrochemical aspects of [RuII(trpy) (pdt)(X)]n+ (trpy = 2,2′:6′,2″-terpyridine, pdt = 5,6-diphenyl-3-pyridyl-as-triazine, X = Cl-, CH3CN, NO2-, NO+, NO.) - electrophilicity of {RuII-NO+} and photolability of {RuII- NO.}

A short and efficient route to δ-lactone-fused cyclopentanoids starting from the easily accessible Diels-Alder adducts between homoallylic alcohol acetates and 1,2,3,4-tetrachloro-5,5-dimethoxycyclopenta-1,3-diene is reported. Since homoallyl alcohols were derived from the corresponding aldehydes RCHO (R = alkyl, aryl) through allyl metal addition, the methodology is broad in scope with regard to the choice of R group. The initially formed 1:1 diastereomeric mixture of adducts were subjected to ruthenium-catalyzed oxidation followed by acid-mediated hydrolysis of the acetate groups to obtain the hemiacetals 6a-e. Alkaline H2O2-mediated cleavage of the hemiacetals led, after esterification with diazomethane, to a chromatographically separable diastereomeric mixture of 7 and 8 in high overall yield (54-68%). © Georg Thieme Verlag Stuttgart.

Synthesis

Synthesis of highly functionalized δ-lactone-fused cyclopentanoids

Nanostructured tungsten oxide (WO3) thin films have been electrochemically grown from a self-assembly of sodium dodecyl sulfate-tungsten oxide aggregates at the electrode-electrolyte interface. The nanoparticulates embedded in a quasi-layered structure of the as-deposited WO3 film with a single-crystalline hexagonal phase transform to a hybrid microstructure encapsulating both nanoscaled particles and rods with a tetragonal modification at 100 °C, reverting again to orthorhombic single-crystalline nanoplatelets and bunches of tangled nanowires at 250 °C and finally coarse nanoparticles at 500 °C. The WO3 film annealed at 100 °C shows the fastest color-bleach kinetics, highest optical modulation and coloration efficiency, which is a repercussion of the pentagonal channels equipped with the tetragonal phase, the mesopore structure and the channeled porosity. In spite of perpendicularly oriented hexagonal channels, which facilitate ion insertion, the switching performance of the as-deposited films comes a close second owing to extremely random pore morphology. Poor color-bleach rates observed for the films annealed at 250 and 500 °C are attributed to pore shrinkage, high density and crystallinity. © 2006 Acta Materialia Inc.