High-performance multifunctional graphene yarns: toward wearable all-carbon energy storage textiles

The successful commercialization of smart wearable garments is hindered by the lack of fully integrated carbon-based energy storage devices into smart wearables. Since electrodes are the active components that determine the performance of energy storage systems, it is important to rationally design and engineer hierarchical architectures atboth the nano- and macroscale that can enjoy all of the necessary requirements for a perfect electrode. Here we demonstrate a large-scale flexible fabrication of highly porous high-performance multifunctional graphene oxide (GO) and rGO fibers and yarns by taking advantage of the intrinsic soft self-assembly behavior of ultralarge graphene oxide liquid crystalline dispersions. The produced yarns, which are the only practical form of these architectures for real-life device applications, were found to be mechanically robust (Young's modulus in excess of 29 GPa) and exhibited high native electrical conductivity (2508 ± 632 S m(-1)) and exceptionally high specific surface area (2605 m(2) g(-1) before reduction and 2210 m(2) g(-1) after reduction). Furthermore, the highly porous nature of these architectures enabled us to translate the superior electrochemical properties of individual graphene sheets into practical everyday use devices with complex geometrical architectures. The as-prepared final architectures exhibited an open network structure with a continuous ion transport network, resulting in unrivaled charge storage capacity (409 F g(-1) at 1 A g(-1)) and rate capability (56 F g(-1) at 100 A g(-1)) while maintaining their strong flexible nature.

Development of high performance materials based on smart elastomer nanocomposites

 The present thesis explores the fabrication of technologically relevant nanocomposites out of a few elastomers and conducting fillers like carbon nanotubes, graphene and polyaniline. The developed materials have good applications in sensors, shape memory devices and capacitors. Different characterization methods reveal the influence of filler-elastomer interactions on the various properties of the obtained nanocomposites as well.

Protocols for finding the most orthogonal dimensions for two-dimensional high performance liquid chromatography

The selection of two high performance liquid chromatography (HPLC) columns with vastly different retention mechanisms is vital for performing effective two-dimensional (2D-) HPLC. This paper reports on a systematic method to select a pair of HPLC columns that provide the most different separations for a given sample. This was completed with the aid of a HPLC simulator that predicted retention profiles on the basis of real experimental data, which is difficult when the contents of sample matrices are largely-or completely-unknown. Peaks from the same compounds must first be matched between chromatograms to compare the retention profiles and optimised 2D-HPLC column selection. In this work, two methods of matching peaks between chromatograms were explored and an optimal pair of chromatography columns was selected for 2D-HPLC. First, a series of 17 antioxidants were selected as an analogue for a coffee extract. The predicted orthogonality of the standards was 39%, according to the fractional surface coverage 'bins' method, which was close to the actual space utilisation of the standard mixture, 44%. Moreover, the orthogonality for the 2D-HPLC of coffee matched the predicted value of 38%. The second method employed a complex sample matrix of urine to optimise the column selections. Seven peaks were confidently matched between chromatograms by comparing relative peak areas of two detection strategies: UV absorbance and potassium permanganate chemiluminescence. It was found that the optimal combinations had an orthogonality of 35% while the actual value was closer to 30%.

High-performance supercapacitor electrode materials from cellulose-derived carbon nanofibers

Nitrogen-functionalized carbon nanofibers (N-CNFs) were prepared by carbonizing polypyrrole (PPy)-coated cellulose NFs, which were obtained by electrospinning, deacetylation of electrospun cellulose acetate NFs, and PPy polymerization. Supercapacitor electrodes prepared from N-CNFs and a mixture of N-CNFs and Ni(OH)2 showed specific capacitances of ∼236 and ∼1045 F g(-1), respectively. An asymmetric supercapacitor was further fabricated using N-CNFs/Ni(OH)2 and N-CNFs as positive and negative electrodes. The supercapacitor device had a working voltage of 1.6 V in aqueous KOH solution (6.0 M) with an energy density as high as ∼51 (W h) kg(-1) and a maximum power density of ∼117 kW kg(-1). The device had excellent cycle lifetime, which retained ∼84% specific capacitance after 5000 cycles of cyclic voltammetry scans. N-CNFs derived from electrospun cellulose may be useful as an electrode material for development of high-performance supercapacitors and other energy storage devices.

Assessing the detectability of antioxidants in two-dimensional high-performance liquid chromatography

This paper explores the analytical figures of merit of two-dimensional high-performance liquid chromatography for the separation of antioxidant standards. The cumulative two-dimensional high-performance liquid chromatography peak area was calculated for 11 antioxidants by two different methods--the areas reported by the control software and by fitting the data with a Gaussian model; these methods were evaluated for precision and sensitivity. Both methods demonstrated excellent precision in regards to retention time in the second dimension (%RSD below 1.16%) and cumulative second dimension peak area (%RSD below 3.73% from the instrument software and 5.87% for the Gaussian method). Combining areas reported by the high-performance liquid chromatographic control software displayed superior limits of detection, in the order of 1 × 10(-6) M, almost an order of magnitude lower than the Gaussian method for some analytes. The introduction of the countergradient eliminated the strong solvent mismatch between dimensions, leading to a much improved peak shape and better detection limits for quantification.

Ex situ electrochemical sodiation/desodiation observation of Co₃O₄ anchored carbon nanotubes: a high performance sodium-ion battery anode produced by pulsed plasma in a liquid

Liquid plasma, produced by nanosecond pulses, provides an efficient and simple way to fabricate a nanocomposite architecture of Co3O4/CNTs from carbon nanotubes (CNTs) and clusters of Co3O4 nanoparticles in deionized water. The crucial feature of the composite's structure is that Co3O4 nanoparticle clusters are uniformly dispersed and anchored to CNT networks in which Co3O4 guarantees high electrochemical reactivity towards sodium, and CNTs provide conductivity and stabilize the anode structure. We demonstrated that the Co3O4/CNT nanocomposite is capable of delivering a stable and high capacity of 403 mA h g(-1) at 50 mA g(-1) after 100 cycles where the sodium uptake/extract is confirmed in the way of reversible conversion reaction by adopting ex situ techniques. The rate capability of the composite is significantly improved and its reversible capacity is measured to be 212 mA h g(-1) at 1.6 A g(-1) and 190 mA h g(-1) at 3.2 A g(-1), respectively. Due to the simple synthesis technique with high electrochemical performance, Co3O4/CNT nanocomposites have great potential as anode materials for sodium-ion batteries.

A highly conductive porous graphene electrode prepared via in situ reduction of graphene oxide using Cu nanoparticles for the fabrication of high performance supercapacitors

Herein, a new graphene/Cu nanoparticle composite was prepared via the in situ reduction of GO in the presence of Cu nanoparticles which was then utilized as a sacrificing template for the formation of flexible and porous graphene capacitor electrodes by the dissolution of the intercalated Cu nanoparticle in a mixed solution of FeCl3 and HCl. The porous RGO electrode was characterized by atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). The as-prepared graphene/Cu nanoparticle composite and the pure graphene film after removal of Cu nanoparticles possessed high conductivity of 3.1 × 10³ S m^-1 and 436 S m^-1 respectively. The porous RGO can be used as the electrode for the fabrication of supercapacitors with high gravimetric specific capacitances up to 146 F g^-1, good rate capability and satisfactory electrochemical stability. This environmentally friendly and efficient approach to fabricating porous graphene nanostructures could have enormous potential applications in the field of energy storage and nanotechnology.

High-performance flexible all-solid-state supercapacitor from large free-standing graphene-PEDOT/PSS films

Although great attention has been paid to wearable electronic devices in recent years, flexible lightweight batteries or supercapacitors with high performance are still not readily available due to the limitations of the flexible electrode inventory. In this work, highly flexible, bendable and conductive rGO-PEDOT/PSS films were prepared using a simple bar-coating method. The assembled device using rGO-PEDOT/PSS electrode could be bent and rolled up without any decrease in electrochemical performance. A relatively high areal capacitance of 448 mF cm(-2) was achieved at a scan rate of 10 mV s(-1) using the composite electrode with a high mass loading (8.49 mg cm(-2)), indicating the potential to be used in practical applications. To demonstrate this applicability, a roll-up supercapacitor device was constructed, which illustrated the operation of a green LED light for 20 seconds when fully charged.

Self-assembled V2O5 interconnected microspheres produced in a fish-water electrolyte medium as a high-performance lithium-ion-battery cathode

Interconnected microspheres of V2O5 composed of ultra-long nanobelts are synthesized in an environmental friendly way by adopting a conventional anodization process combined with annealing. The synthesis process is simple and low-cost because it does not require any additional chemicals or reagents. Commercial fish-water is used as an electrolyte medium to anodize vanadium foil for the first time. Electron microscopy investigation reveals that each belt consists of numerous nanofibers with free space between them. Therefore, this novel nanostructure demonstrates many outstanding features during electrochemical operation. This structure prevents self-aggregation of active materials and fully utilizes the advantage of active materials by maintaining a large effective contact area between active materials, conductive additives, and electrolyte, which is a key challenge for most nanomaterials. The electrodes exhibit promising electrochemical performance with a stable discharge capacity of 227 mAh·g–1 at 1C after 200 cycles. The rate capability of the electrode is outstanding, and the obtained capacity is as high as 278 at 0.5C, 259 at 1C, 240 at 2C, 206 at 5C, and 166 mAh·g–1 at 10C. Overall, this novel structure could be one of the most favorable nanostructures of vanadium oxide-based cathodes for Li-ion batteries. [Figure not available: see fulltext.]

High performance green buildings

This work aims to study and analyze strategies and measures to improve energy performance in residential and service buildings, in order to minimize energy losses and energy consumption. Due to the high energy dependence of European Union (EU), including Portugal and Slovenia, and high percentage of energy consumption in the building sector, there was a need to adopt strategies at European level with ambitious goals. This came to force EU - Member States to take measures to achieve the proposed targets for energy consumption reduction. To this end, EU - Member States have adapted the laws to their needs and formed specialized agencies and qualified experts on energy certification, which somehow evaluate buildings according to their performance. In this study, the external characteristics of the building in order to meet its thermal needs and from there to survey the existing and possible constructive solutions to be used at the envelope will be examined, in order to increase comfort and reduce the need of use technical means of air conditioning. The possibility of passive heating and ventilation systems also will be discussed. These techniques are developed in parallel with the deployment and design of the building. In this manner, to reduce the energy consumption, various techniques and technologies exploit natural resources. Thus, appear the more sustainable and efficient buildings, so-called Green Buildings have been appeared. The study ends with the identification of measures used in several buildings, proving the economic return in the medium to long term, as well as the satisfaction of their users.

A fast method using a new hydrophilic–lipophilic balanced sorbent in combination with ultra-high performance liquid chromatography for quantification of significant bioactive metabolites in wines

This manuscript describes the development and validation of an ultra-fast, efficient, and high throughput analytical method based on ultra-high performance liquid chromatography (UHPLC) equipped with a photodiode array (PDA) detection system, for the simultaneous analysis of fifteen bioactive metabolites: gallic acid, protocatechuic acid, (−)-catechin, gentisic acid, (−)-epicatechin, syringic acid, p-coumaric acid, ferulic acid, m-coumaric acid, rutin, trans-resveratrol, myricetin, quercetin, cinnamic acid and kaempferol, in wines. A 50-mm column packed with 1.7-μm particles operating at elevated pressure (UHPLC strategy) was selected to attain ultra-fast analysis and highly efficient separations. In order to reduce the complexity of wine extract and improve the recovery efficiency, a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a new macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis™ HLB), was performed prior to UHPLC–PDA analysis. The calibration curves of bioactive metabolites showed good linearity within the established range. Limits of detection (LOD) and quantification (LOQ) ranged from 0.006 μg mL−1 to 0.58 μg mL−1, and from 0.019 μg mL−1 to 1.94 μg mL−1, for gallic and gentisic acids, respectively. The average recoveries ± SD for the three levels of concentration tested (n = 9) in red and white wines were, respectively, 89 ± 3% and 90 ± 2%. The repeatability expressed as relative standard deviation (RSD) was below 10% for all the metabolites assayed. The validated method was then applied to red and white wines from different geographical origins (Azores, Canary and Madeira Islands). The most abundant component in the analysed red wines was (−)-epicatechin followed by (−)-catechin and rutin, whereas in white wines syringic and p-coumaric acids were found the major phenolic metabolites. The method was completely validated, providing a sensitive analysis for bioactive phenolic metabolites detection and showing satisfactory data for all the parameters tested. Moreover, was revealed as an ultra-fast approach allowing the separation of the fifteen bioactive metabolites investigated with high resolution power within 5 min.

Determination of gatifloxacin in bulk and tablet preparations by high-performance liquid chromatography

A sensitive, precise, and specific high-performance liquid chromatographic (HPLC) method was developed for the assay of gatifloxacin (GATX) in raw material and tablets. The method validation parameters yielded good results and included the range, linearity, precision, accuracy, specificity, and recovery. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The HPLC separation was carried out by reversed-phase chromatography on a C18 absorbosphere column (250 x 4.6 mm id, 5 pm particle size) with a mobile phase composed of acetic acid 50/o--acetonitrile-methanol (70 + 15 + 15, v/v/v) pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 287 nm. The calibration graph for GATX was linear from 4.0 to 14.0 mu g/mL. The interday and intraday precisions (relative standard deviation) were less than 1.05%.

High-performance liquid chromatographic determination of amfepramone hydrochloride, mazindol, and diazepam in tablets

Simple and rapid procedures were developed for the quantification of amfepramone hydrochloride and diazepam and mazindol and diazepam in tablets using high performance liquid chromatography (HPLC) with UV detection. These techniques provided conditions for the separation of each active ingredient from the complex matrices of the dosage forms by dilution or extraction in methanol. Isocratic reversed phase chromatography was performed using acetonitrile, methanol, and aqueous 0,1% ammonium carbonate (70:10:20, v/v/v) as a mobile phase, Radial-Pak C-18 column (100 x 8 mm id, 4 mu m), a column temperature of 25+/-1 degrees C and detection at 255 nm. The calibration curves were linear over a wide concentration range (100-1000 mu g.mL(-1) to amfepramone hydrochloride and mazindol and 10-100 mu g.mL(-1) to diazepam) with good correlation factors of 0.9978, 0.9956 and 0.9997 for amfepramone hydrochloride, mazindol, and diazepam, respectively.Mean recoveries obtained from the two kinds of samples ranged from 83.2 to 102.5%, with coefficients of variation ranging from 1.0 to 6.1.These results demonstrated the efficiency of the proposed methods, as well as advantages such as simplicity and short duration of analysis.

Identification of oligomers in polyethyleneterephthalate bottles for mineral water and fruit juice - Development and validation of a high-performance liquid chromatographic method for the determination of first series cyclic trimer

Cyclic oligomers were identified in PET bottles used for mineral water and fruit juice using MS and H-1 and C-13 NMR: a first series cyclic trimer, a first series cyclic tetramer, a first series cyclic dimmer and a second series cyclic trimer. An analytical method to determine first series cyclic trimer in these bottles was developed and validated, using HPLC. The first series cyclic trimer levels were 316-462 mg/100 g of PET bottle. (c) 2005 Elsevier B.V. All rights reserved.