Concomitant use of liquid–liquid batch and continuous plug flow reactors for kinetic model discrimination. Application to the Rh/TPPTS catalysed reduction of the C–C double bond in dimethylitaconate

The biphasic catalytic reduction of the C–C double bond of dimethylitaconate with a water soluble rhodium/triphenylphosphinetrisulphonated sodium salt (TPPTS) complex is investigated. Kinetic studies in a well-mixed batch reactor provide kinetics parameters and an activation energy of 71 kJ mol⁻¹ but cannot discriminate between a first order or a complex kinetic model within the range of substrate concentration where the approximation of linear liquid/liquid partition is respected. Catalytic tests in the centrifugal partition chromatograph (CPC) reactor under steady-state operations in chemical regime and plug flow mode allow discriminating the kinetic models, the complex kinetic rate law being preferred.     

Valorization of Beef Tallow by Lipase-Catalyzed Interesterification with High Oleic Sunflower Oil

Although beef tallow (BT) has been considered a hard low-trans fat convenient to be used in several bakery applications, it has some undesirable characteristics like fatty acid composition, crystallization behavior, graininess formation and poor plastic range. This work studied the modification of BT by blending at different percentages with high oleic sunflower oil (HOSFO) followed by the enzyme-catalyzed interesterification of the blends. The reduction in the solid fat content achieved by the simple blending was enhanced by the interesterification process, as a result of the increase in the concentration of the diunsaturated monosaturated type triacylglycerols. Interesterification strongly impacted too on the crystallization behavior of the blends, since products showed more homogeneous and regular crystals than the starting mixture. Results show that lipase catalyzed interesterification of BT with HOSFO offers a useful tool for the design of fats with adjustable physicochemical properties, improved with respect to that of the starting fats.     

Application of power addition as modelling technique for flow processes: Two case studies

In many of the continuum processes typically found in chemical engineering, the functional dependency of the dependent variable is only known for large and small values of the independent variable. Exact solutions in the transitional regime are often obscure for various reasons (e.g. narrow band within which the transition from one regime to the other occurs, inadequate knowledge of the physics in this area, etc.). An established method for the matching of limiting solutions is reviewed and subsequently applied. The method regards the known solutions as asymptotes and proposes addition to a power of such asymptotes. It yields a single, adjustable correlating equation that is applicable over the entire domain. This procedure circumvents the introduction of ad hoc curve fitting measures for the different regions and subsequent, unwanted discontinuities in piece-wise fitted correlative equations for the dependent variables. Experimental data of two diverse processes, namely flow in a straight-through diaphragm valve and the fluidisation of a packed bed, are analysed as case studies. Empirical results are investigated for possible asymptotic bounds whereafter power addition is applied to the functional dependencies. The outcome is compared to those of the empirical models and the results discussed. The procedure is revealed to be highly useful in the summarising and interpretation of experimental data in an elegant and simplistic manner. It may also, in general, aid the setup of experimental apparatus for investigation of continuum processes.     

Molecular absorption spectrophotometric method for the determination of phosphorus in biodiesel

A molecular absorption method is proposed for the determination of phosphorus in biodiesel. The samples are mineralized using an ashing procedure at 550 °C followed by dissolution of the residue. The analytical procedure is based on the formation of a blue molybdenum complex. 1-amino-2-naphthol-4-sulfonic acid is used as reducing agent. The method was applied to biodiesel samples prepared from soy, canola and sunflower oils and from bovine fat. The limit of detection is 0.57 mg P kg⁻¹ and the limit of quantification is 1.7 mg P kg⁻¹. The observed mean relative standard deviation is about 5%. The simplicity of the procedure added to its precision, accuracy and low cost suggest that it is an excellent option for the determination of phosphorus in biodiesel.     

Synthesis,characterization and evaluation of phosphorylated resins in the removal of Pb<Superscript>2+</Superscript> from aqueous solutions

Phosphinic-derivative poly(styrene-co-divinylbenzene)-based on PS–DVB copolymers with different porosity degrees have been prepared by aromatic electrophilic substitution reaction using PCl₃/AlCl₃ followed by base-promoted hydrolysis. The phosphorylation reaction was analyzed by infra-red spectroscopy (FTIR), scanning electron microscopy (SEM), and thermogravimetry (TG/DTG). In addition, the phosphorous content of the phosphorylated copolymers was determined by spectrophotometry using the method based on sodium molybdate reactant so that the extension of that modification could be assessed. The performance of the phosphorylated resins in the extraction of Pb²⁺ from aqueous solutions in a batch system was also evaluated. The Pb²⁺ content was determined by atomic absorption spectrometry (AAS). These materials presented excellent extraction capacity under the contact time of 30 min and pH 6.     

Ultra Low Background Cryogenic Test Facility for Far-Infrared Radiation Detectors

The next generation of far infrared radiation detectors is aimed to reach photon noise limited performance in space based observatories such as SPICA and BLISS. These detectors operate at loading powers of the astronomical signal of a few Attowatt (10^?18 W) or less, corresponding to a sensitivity expressed in noise equivalent power as low as $\mathrm{NEP} = 2\times10^{-20}\ \mbox{W}/\sqrt{\mathrm{Hz}}$ . We have developed a cryogenic test setup for microwave Kinetic Inductance Detectors (MKIDs) that aims to reach these ultra-low background levels. Stray light is stopped by using a box in a box design with a sample holder inside another closed box. Microwave signals for the MKID readout enters the outer box through custom made coax cable filters. The stray light loading per pixel is estimated to be less than 60×10^?18 W during nominal operation, a number limited by the intrinsic sensitivity of the MKIDs used to validate the system.     

An 8-b 650-MHz folding ADC

An 8-b 650-MHz folding analog-to-digital converter (ADC) with analog error correction in the comparators is presented. With an input frequency of 150 MHz, 7.8 effective bits are obtained. The ADC is implemented in a 1-μm 13-GHz triple-level interconnect bipolar process, requiring 850 mW from a single -4.5 V supply. The die size is 4.2 mm²