Thermal conductivity and Kapitza resistance of cyanate ester epoxy mix and tri-functional epoxy electrical insulations at superfluid helium temperature

In the framework of the European Union FP7 project EuCARD, two composite insulation systems made of cyanate ester epoxy mix and tri-functional epoxy (TGPAP-DETDA) with S-glass fiber have been thermally tested as possible candidates to be the electrical insulation of 13 T Nb₃Sn high field magnets under development for this program. Since it is expected to be operated in pressurized superfluid helium at 1.9 K and 1 atm, the thermal conductivity and the Kapitza resistance are the most important input parameters for the thermal design of this type of magnet and have been determined in this study. For determining these thermal properties, three sheets of each material with different thicknesses varying from 245 to 598 μm have been tested in steady-state condition in the temperature range of 1.6–2.0 K. The thermal conductivity for the tri-functional epoxy (TGPAP-DETDA) epoxy resin insulation is found to be k = [(34.2 ± 5.5)?T ? (16.4 ± 8.2)] × 10^?3 Wm^?1 K^?1 and for the cyanate ester epoxy k = [(26.8 ± 4.8)?T ? (9.6 ± 5.2)] × 10^?3 Wm^?1 K^?1. For the Kapitza resistance, R_k, the best curve fitting the experimental data is described by R_k = (3057 ± 593) × 10^?6?T (?1.79 ± 0.34) m² KW^?1 for the TGPAP-DETDA insulation and R_k = (4114 ± 971) × 10^?6?T (?1.73 ± 0.41) m² KW^?1 for the cyanate ester epoxy insulation. Our results are compared with other epoxy based composite electrical insulation found in the literature.     

Estimation of diffusion parameters in fluidized bed drying

The present work is an attempt to assess the drying kinetics of green pepper in a fluidized bed in a temperature range of 65–105 °C. The drying kinetics is modeled using several semi empirical models to estimate the kinetic parameters. Although the semi empirical model could fit the experimental data well within acceptable experimental error limits, the two parameter models such as Henderson Pabis model and Page Model are identified to predict the drying kinetics with lesser error. The kinetic parameter (k) is found to increase with the temperature for all the models. The activation energy (E) estimated using Arrhenius equation is found to be 30.3 kJ/mol, while the Arrhenius constant (k_o) is found to be 0.09 s^?1. The effective diffusivity coefficient is evaluated using Fick’s diffusion equation which is found increase with increase in temperature of the heating medium and to vary from 1.95 × 10^?11 to 7 × 10^?11 m²/s.     

Potentiometric determination of ketoprofen and piroxicam at a new PVC electrode based on ion associates of Rhodamine 6G

The characteristics, performance and application of ion-selective electrodes for ketoprofen and piroxicam ions based on Rhodamine 6G as electrode-active substances are described. These electrodes respond with sensitivities of (58.0 ± 1.0) and (57.0 ± 2.0) mV/decade over the range 1.0 × 10^? 4–1.0 × 10^? 1 and 1.0 × 10^? 4–5.0 × 10^? 2 mol/l at pH 5–9 and 6–10 and a detection limit of 6.3 × 10^? 5 and 3.2 × 10^? 5 mol/l for ketoprofen and piroxicam, respectively. The electrodes are easily constructed at a relatively low cost, have a fast response time and can be used for a period of 5 months without any considerable divergence in potential. The proposed sensor displayed good selectivity for ketoprofen and piroxicam in the presence of several substances and inorganic anions. It was used for the direct assay of ketoprofen and piroxicam in commercial pharmaceutical preparations.     

Iodide selective membrane electrodes based on a Molybdenum–Salen as a neutral carrier

A new polymeric membrane electrode (PME) and a coated platinum disk electrode (CPtE) based on Schiff base complex of Mo(VI) as a suitable carrier for I^? ion were described. The influence of membrane composition, pH and possible interfering anions were investigated on the response properties of the electrodes. The electrodes exhibited a Nernstian slope of 63.0 ± 0.5 (CPtE) and 60.3 ± 0.4 (PME) mV decade^? 1 in I^? ion over a wide concentration range from 7.9 × 10^? 7 to 1.0 × 10^? 1 M for CPtE and 9.1 × 10^? 6 to 1.0 × 10^? 1 M I^? for PME. The potentiometric response of the electrodes was independent of the pH of the test solution in the pH range 2.0–8.5 with a fast response time (< 10 s). The process of transfer of iodide across the membrane interface was investigated by use of the AC impedance technique. The proposed sensors were successfully applied to direct determination of iodide in samples containing interfering anions, waste water and as indicator electrodes in precipitation titrations.     

Thermal expansion of hydroxyapatite between − 100 °C and 50 °C

Hydroxy apatite (HAp) ceramic was synthesized using traditional sintering. Dilatometric and lattice thermal expansion properties of a HAp ceramic were evaluated at temperatures of ? 100–50 °C. In that temperature range, the dilatometric thermal expansion coefficient and the lattice thermal expansion coefficient of the HAp ceramic were, respectively, 10.6 × 10^? 6/°C and 9.9 × 10^? 6/°C. Furthermore, thermal expansion properties of a human tooth were measured. The thermal expansion coefficient of the horizontal direction perpendicular to the growing direction of a tooth was 15.5 × 10^? 6/°C; that of the vertical direction along with the direction of tooth growth was 18.9 × 10^? 6/°C at the temperature range described above.     

A reference specimen for permeability measurements of fibrous reinforcements for RTM

The capability to simulate the flow of resin through a porous reinforcement by FE modelling has become very important for designing RTM production processes for high-performance composite parts. The key parameter in RTM flow simulations is the fibre reinforcement permeability. The measurement of this material parameter is still not standardized and many different set-ups have been proposed. Recently, a stereolithography technique was used to produce a textile-like solid specimen with anisotropic permeability, designed as a reference for calibration and comparison of permeability measurement set-ups and for validation of numerical permeability computation software. Unlike real textiles, the permeability properties of such reference specimens do not vary from test to test. Excellent repeatability of the experiments is achieved. When used for benchmarking, any discrepancy between different measurements on this specimen must be attributed to the set-up and data processing.This paper presents the first experimental measurements of the permeability of such reference specimens, obtained with a 2D central injection rig. The measured values, with principal components of the 2D permeability tensor of 2.47 ± 0.09 × 10^?9 m² and 5.44 ± 0.22 × 10^?9 m², are in good agreement with the values predicted using numerical permeability computation software. Statistics from a series of measurements using the same set-up show that the precision of the permeability identification depends on the data processing procedure. An approach which incorporates a numerical model that is also valid after the fluid reached an edge of the reinforcement performs significantly better than the approach, based on an analytical approximation, which was used before.     

Selective electrodes for [PF6]− and [BF4]− anions based on the associates formed by ionic liquid and cationic dyes

The feasibility of the newly synthesized ionic associates L1 and L2 formed by ionic liquid [C₄mim][PF₆] and cationic dyes (malachite green and methylene blue) has been tested as a novel ionophore for the preparation of anion-selective polymeric membrane electrodes. The electrode exhibits Nernstian response and enhanced potentiometric selectivity towards [PF₆]^? compared to many other anions. The influence of some experimental parameters such as membrane composition, nature of plasticizer and amount of additive on the potential response of the [PF₆]^? sensor are investigated. Under the optimized conditions, the response slopes of the membrane electrodes towards [PF₆]^? are 59.7 ± 0.5 and 58.1 ± 0.5 mV/decade based on ionophore L1 and L2, respectively, in 1.0 × 10^? 5–1.0 × 10^? 1 or 1.0 × 10^? 6–1.0 × 10^? 1 mol/L concentration range. Interestingly, the optimized electrodes based on ionophores L1 and L2 also exhibit Nernstian response characteristics (60.3 ± 0.5 and 56.0 ± 0.5 mV/decade) for tetrafluoroborate anion [BF₄]^? in a wide concentration range. Thus, the proposed sensor has been used for the determination of [PF₆]^? and [BF₄]^? in aqueous ionic liquids samples and the solubility of the [PF₆]^? and [BF₄]^? based ionic liquids in water. The satisfactory results are obtained.     

Synthesis of hydroxyapatite crystals using carboxymethyl inulin for use as a delivery of ibuprofen

In the present study biodegradable, environmentally friendly polysaccharide-based polycarboxylate, carboxymethyl inulin (CMI), was used to produce hydroxyapatite (HAP) particles by wet chemical synthesis under controlled temperature, pH, and atmospheric conditions. The morphology and microstructure of the HAP nanoparticles were investigated by XRD, SEM, DTA–TGA and FTIR. CMI affects morphology, surface area, dimension and particle size distribution of the crystals. The reduction in size is greater in the direction of the c-axis. The increase in the polymer concentration to 7.5 g/L resulted in the mixture of nanoparticles with particle sizes of less than 100 nm. The SEM micrograph shows the formation of well-crystallized, agglomerated small particles of HAP. X-ray analysis has shown that the resulting particles have high thermal stability.The obtained crystals were used to produce tablets by direct compression of HAP. The influence of sample's CMI concentration on drug release profiles was investigated by using ibuprofen (C₁₃H₁₈O₂) as a model drug. The model was used to determine the effective diffusion coefficient of the drug from the tablets. A good agreement between experimental data and model predictions was obtained as calculated in the present work. The values of the diffusion coefficients range from 1.62 × 10^? 7 to 4.72 × 10^? 7 m² h^? 1.     

Determination of benzalkonium chloride preservative in pharmaceutical formulation of eye and ear drops using new potentiometric sensors

A novel approach for determination of low concentrations of the preservative, benzalkonium chloride (BCCl), in pharmaceutical formulation constitutes is presented. New chemically modified carbon paste electrodes (CMCPEs) are developed. The first is based on an ion-association of BCCl with phosphomolybdic acid (PMA) as the ion-exchanger (BC–PM) dissolved in the mixed plasticizers dibutyl phthalate (DBP) and dioctyl sebacate (DOS) encoded sensor A. In the other electrode, encoded sensor B, the plasticizers DBP and dioctyl phthalate (DOP) are more suitable solvent mediators for the paste. These electrodes exhibit a Nernstian slope of 58.2 ± 0.6 and 62.3 ± 0.7 mV/decade in concentration range 1.3 × 10^? 7–1.7 × 10^? 4 M and 2.5 × 10^? 7–1.7 × 10^? 4 M with the limit of detection of 1.0 × 10^? 7 M and 1.6 × 10^? 7 for sensors A and B, respectively. The sensors have short and stable response time 5–8 s, good reproducibility and can be used in pH range of 5.7–8.6. The present electrodes show good discrimination of BCCl from several inorganic, organic ions and some common drug excipients. These characteristics of the electrodes make them useful in successful determination of BCCl in its pharmaceutical preparations (eye and ear drops) and aqueous solutions. The results obtained were satisfactory with excellent percentage recovery comparable and sometimes better than those obtained by other routine methods for the assay.     

An innovative process to fabricate copper/diamond composite films for thermal management applications

Diamond dispersed copper matrix (Cu/D) composite films with strong interfacial bonding were produced by tape casting and hot pressing without carbide forming additives. The tape casting process offers an original solution to obtain laminated materials with accurate thickness control, smooth surface finish, material net-shaping, scalability, and low cost. This study presents an innovative process of copper submicronic particles deposition onto diamond reinforcements prior to densification by hot pressing. Copper particles act as chemical bonding agents between the copper matrix and the diamond reinforcements during hot pressing, thus offering an alternative solution to traditionnal carbide-forming materials in order to get efficient interfacial bonding and heat-transfer in Cu/D composites. It allows high thermal performances with low content of diamond, thus enhancing the cost-effectiveness of the materials. Microstructural study of composites by scanning electron microscopy (SEM) was correlated with thermal conductivity and thermal expansion coefficient measurements. The as-fabricated films exhibit a thermal conductivity of 455 W m^?1 K^?1 associated to a coefficient of thermal expansion of 12 × 10^?6 °C^?1 and a density of 6.6 g cm^?3 with a diamond volume fraction of 40%, which represents a strong enhancement relative to pure copper properties (λ_Cu = 400 W m^?1 K^?1, α_Cu = 17 × 10^?6 °C^?1, ρ_Cu = 8.95 g cm^?3). The as-fabricated composite films might be useful as heat-spreading layers for thermal management of power electronic modules.     

Electrocatalytical oxidation and sensitive determination of acetaminophen on glassy carbon electrode modified with graphene–chitosan composite

The electrochemical behaviors of acetaminophen (ACOP) on a graphene–chitosan (GR–CS) nanocomposite modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), chronocoulometry (CC) and differential pulse voltammetry (DPV). Electrochemical characterization showed that the GR–CS nanocomposite had excellent electrocatalytic activity and surface area effect. As compared with bare GCE, the redox signal of ACOP on GR–CS/GCE was greatly enhanced. The values of electron transfer rate constant (k_s), diffusion coefficient (D) and the surface adsorption amount (Γ^?) of ACOP on GR–CS/GCE were determined to be 0.25 s^? 1, 3.61 × 10^? 5 cm² s^? 1 and 1.09 × 10^? 9 mol cm^? 2, respectively. Additionally, a 2e^?/2H⁺ electrochemical reaction mechanism of ACOP was deduced based on the acidity experiment. Under the optimized conditions, the ACOP could be quantified in the range from 1.0 × 10^? 6 to 1.0 × 10^? 4 M with a low detection limit of 3.0 × 10^? 7 M based on 3S/N. The interference and recovery experiments further showed that the proposed method is acceptable for the determination of ACOP in real pharmaceutical preparations.     

Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag⁺ ion ranging from 1.0 × 10^? 6 to 1.0 × 10^? 1 M with a detection limit of 9.5 × 10^? 7 M and a slope of 60.4 ± 0.2 mV dec^? 1 over a wide pH range (4.0–9.0) with a fast response time (50 s) at 25 °C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl^? and Br^? ions.     

A new silver(I)-selective electrode based on derivatized MWCNTs@SiO2 nanocomposites as a neutral carrier

For the first time a novel carbon paste electrode (CPE) for the detection of trace silver(I) was designed by using derivatized silica-coated multi-walled carbon nanotubes (MWCNTs@SiO₂) nanocomposites as a neutral carrier. This proposed electrode, with optimum composition, exhibits a wide dynamic range of 8.6 × 10^? 8 to 1.0 × 10^? 1 M toward silver(I) with a detection limit of 8.0 × 10^? 8 M and a Nernstian slope of 60.8 ± 0.2 mV dec^? 1. Meanwhile, it also shows a good selectivity and a relatively fast response time (~ 20 s), a long lifetime (1 month) and a wide pH range (4.0–9.0). Finally, the developed CPEs were successfully applied in the potentiometric titration of potassium bromide and determination of Cl^? ions in different water samples.     

Application of nanostructured ZnO films for electrochemical DNA biosensor

Nanostructured zinc oxide (nsZnO) films have been fabricated onto conducting indium–tin–oxide (ITO) coated glass plate, by cathodic electro-deposition to immobilize probe DNA specific to M. tuberculosis via physisorption based on strong electrostatic interactions between positively charged ZnO (isoelectric point = 9.5) and negatively charged DNA to detect its complementary target. Electrochemical studies reveal that the presence of nano-structured ZnO results in increased electro-active surface area for loading of DNA molecules. The DNA–nsZnO/ITO bioelectrode exhibits interesting characteristics such as detection range of 1 × 10^?6 ? 1 × 10^?12 M, detection limit of 1 × 10^?12 M (complementary target) and 1 × 10^?13 M (genomic DNA), reusability of about 10 times, response time of 60s and stability of up to 4 months when kept at 4°C.     

High-precision CTE measurement of hybrid C/SiC composite for cryogenic space telescopes

This paper presents highly precise measurements of thermal expansion of a “hybrid” carbon-fiber reinforced silicon carbide composite, HB-Cesic® – a trademark of ECM, in the temperature region of ～310–10 K. Whilst C/SiC composites have been considered to be promising for the mirrors and other structures of space-borne cryogenic telescopes, the anisotropic thermal expansion has been a potential disadvantage of this material. HB-Cesic® is a newly developed composite using a mixture of different types of chopped, short carbon-fiber, in which one of the important aims of the development was to reduce the anisotropy. The measurements indicate that the anisotropy was much reduced down to 4% as a result of hybridization. The thermal expansion data obtained are presented as functions of temperature using eighth-order polynomials separately for the horizontal (XY-) and vertical (Z-) directions of the fabrication process. The average CTEs and their dispersion (1σ) in the range 293–10 K derived from the data for the XY- and Z-directions were 0.805 ± 0.003 × 10^?6 K^?1 and 0.837 ± 0.001 × 10^?6 K^?1, respectively. The absolute accuracy and the reproducibility of the present measurements are suggested to be better than 0.01 × 10^?6 K^?1 and 0.001 × 10^?6 K^?1, respectively. The residual anisotropy of the thermal expansion was consistent with our previous speculation regarding carbon-fiber, in which the residual anisotropy tended to lie mainly in the horizontal plane.     

Mechanical properties,urea diffusion,and cell cultural response of poly(vinyl alcohol)–Chitosan bioartificial membranes via molecular modelling and experimental investigation

An in silico protocol jointly with experimental approach is here used to design and investigate poly(vinyl alcohol) (PVA)–Chitosan polymer membranes. Atomistic computational investigations were performed to assess mechanical behaviour and urea molecules diffusion of PVA–Chitosan blend bulk models with different compositions. Blend membranes of PVA–Chitosan were prepared with different compositions by solvent-casting technique and their swelling behaviour, morphological, mechanical and transport properties were investigated. Cytotoxicity assessments by means of in vitro, indirect contact assay were carried using L929 fibroblast-like cells. The values of the Young modulus along the three perpendicular directions of computational systems were very similar and ranged from 3.64 to 4.39 GPa. Urea diffusivity was related to the blends composition and the values ranged from 1.62 × 10^?7 to 9.56 × 10^?8 cm²/s. Overall, a good agreement was found between experimental and simulation data.     

New potentiometric sensor for the determination of iodine species

The characteristics, performance and application of novel triiodide potentiometric sensor based on ion-pair of Rhodamine B triiodide as a membrane carrier are described. The electrode has a linear dynamic range between 1 × 10^? 6 and 1 × 10^? 1 M, with a Nernstian slope of 68 ± 1 mV pC^? 1 and detection limit of 3.9 × 10^? 7 M. Fast and stable response, good reproducibility, long-term stability, very good selectivity over a large number of common organic and inorganic anions, applicability over a pH range of 2–10 are demonstrated. The proposed sensor has been applied for potentiometric determination of some iodine species.     

Electrochemical hydrogen evolution of multi-walled carbon nanotube/micro-hybrid composite decorated with Ni nanoparticles as catalyst through electroless deposition process

Hydrogen evolution of multi-walled nanotube (MWCNT)/micro-hybrid polymer composite, decorated with Ni nanoparticles through electroless deposition process is studied by the electrochemical method. Cyclic voltammetry (CV) is utilized to clearly study the electrochemical hydrogen storage/evolution behavior of the composite through a potential window ranging from ? 1.60 to + 0.60 V (vs. Ag/AgCl). Hydrogen adsorption/desorption peaks are positioned at ? 1.52 and ? 0.05 V, respectively. Chronoamperometry is also applied to estimate active surface area (0.145 m² g^? 1) of the composite as well as the diffusion coefficient (3.4 × 10^? 11 m² s^? 1) of adsorbed hydrogen process. According to the chrono-charge/discharge technique, the capacity of fabricated Ni-MWCNT/micro-hybrid composite is estimated to be 2.98 wt.% during charging for a certain time (40 min).     

Fabrication of a PVC membrane samarium(III) sensor based on N,N′,N″-tris(4-pyridyl)trimesic amide as a selectophore

A new ion-selective electrode for Sm^3 + ion is described based on the incorporation of N,N′,N″-tris(4-pyridyl)trimesic amide (TPTA) in a poly(vinylchloride) (PVC) matrix. The membrane sensor comprises nitrobenzene (NB) as a plasticizer, and oleic acid (OA) as an anionic additive. The sensor with the optimized composition shows a Nernstian potential response of 19.8 ± 0.5 mV decade^? 1 over a wide concentration range of 1.0 × 10^? 2 and 1 × 10^? 6 mol L^? 1, with a lower detection limit of 4.7 × 10^? 7 mol L^? 1 and satisfactor applicable pH range of 3.6–9.2. Having a short response time of less than 10 s and a very good selectivity towards the Sm^3 + over a wide variety of interfering cations (e.g. alkali, alkaline earth, transition and heavy metal ions) the sensor seemed to be a promising analytical tool for determination of the Sm^3 +. Hence, it was used as an indicator electrode in the potentiometric titration of samarium ion with EDTA. It was also applied to the direct samarium recovery in binary mixtures.     

An optical chemical sensor for thorium (IV) determination based on thorin

A selective method for the determination of thorium (IV) using an optical sensor is described. The sensing membrane is prepared by immobilization of thorin–methyltrioctylammonium ion pair on triacetylcellulose polymer. The sensor produced a linear response for thorium (IV) concentration in the range of 6.46 × 10^?6 to 9.91 × 10^?5 mol L^?1 with detection limit of 1.85 × 10^?6 mol L^?1. The regeneration of optode was accomplished completely at a short time (less than 20 s) with 0.1 mol L^?1 of oxalate ion solution. The relative standard deviation for ten replicate measurements of 2.15 × 10^?5 and 8.62 × 10^?5 mol L^?1 of thorium was 2.71 and 1.65%, respectively. The optode membrane exhibits good selectivity for thorium (IV) over several other ionic species and are comparable to those obtained in case of spectrophotometric determination of thorium using thorin in solution. A good agreement with the ICP-MS and spiked method was achieved when the proposed optode was applied to the determination of thorium (IV) in dust and water samples.