A simple differential titrator for automatic potentiometric titration at zero current, with two identical indicator electrodes

A simple differential titrator for automatic potentiometric titration at zero current, with two identical indicator electrodes, is described. The autoburette is a normal microburette connected to one tube of a peristaltic pump, and the differentiating system is a closed-flow circuit in a second tube of the pump, this tube containing two electrodes 5 cm apart. The apparatus has been applied to the determination of halides and sulphide-disulphide mixtures, with electrodes coated with an appropriate silver salt.     

Ferrocenyl-substituted α,β-unsaturated ketones in synthesis of tetrahydropyrimidinones

Ferrocenyltetrahydropyrimidin-2-ones were prepared by reactions of linear and cyclic ,-unsaturated ketones of the ferrocene series with urea in i-PrOH in the presence of t-BuOK. The structures of the compounds prepared were studied by ¹H and ¹³C NMR and IR spectroscopy, and also by single crystal X-ray diffraction.Translated from Zhurnal Obshchei Khimii, Vol. 74, No. 11, 2004, pp. 1887–1893.Original Russian Text Copyright © 2004 by E. Klimova, Lorez, T. Klimova, Garcia, Hernandez, Ramirez.This revised version was published online in April 2005 with a corrected cover date.     

Silicon‐containing trifunctional and tetrafunctional cyanate esters: Synthesis,cure kinetics,and network properties

The synthesis and physical properties of new silicon‐containing polyfunctional cyanate ester monomers methyl[tris(4‐cyanatophenyl)]silane and tetrakis(4‐cyanatophenyl)silane, as well as polycyanurate networks formed from these monomers are reported. The higher crosslinking functionality compared to di(cyanate ester) monomers enables much higher ultimate glass transition temperatures to be obtained as a result of thermal cyclotrimerization. The ability to reach complete conversion is greatly enhanced by cocure of the new monomers with di(cyanate ester) monomers such as 1,1‐bis(4‐cyanatophenyl)ethane. The presence of silicon in these polycyanurate networks imparts improved resistance to rapid oxidation at elevated temperatures, resulting in char yields as high as 70% under nitrogen and 56% in air in the best‐performing networks. The water uptake in the silicon‐containing networks examined is 4–6 wt % after 96 h of immersion at 85 °C, considerably higher than both carbon‐containing and/or di(cyanate ester) analogs. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 767–779     

Longitudinal 3D Blood Flow Distribution Provided by Diffuse Correlation Tomography during Bone Healing in a Murine Fracture Model

Noninvasive monitoring of vascularization can potentially diagnose impaired bone healing earlier than current radiographic methods. In this study, a noncontact diffuse correlation tomography (DCT) technique was employed to measure longitudinal blood flow changes during bone healing in a murine femoral fracture model. The three-dimensional distribution of the relative blood flow was quantified from one day pre-fracture to 48 days post-fracture. For three mice, frequent DCT measurements were performed every other day for one week after fracture, and then weekly thereafter. A decrease in blood flow was observed in the bone fracture region at one day post-fracture, followed by a monotonic increase in blood flow beyond the pre-injury baseline until five to seven days post-fracture. For the remaining 12 mice, only weekly DCT measurements were performed. Data collected on a weekly basis show the blood flow for most mice was elevated above baseline during the first two post-fracture weeks, followed by a subsequent decrease. Torsional strength of the excised femurs was measured for all 15 mice after 7 weeks of healing. A metric based on the early blood flow changes shows a statistically significant difference between the high strength group and the low strength group.     

New palladium (II) complexes containing phosphine‐nitrogen ligands and their use as catalysts in aminocarbonylation reaction

Aminocarbonylation of aryl halides, homogeneously catalysed by palladium, is an efficient method that can be employed for obtaining amides for pharmaceutical and synthetic applications. In this work, palladium (II) complexes containing P^N ligands were studied as catalysts in the aminocarbonylation of iodobenzene in the presence of diethylamine. Two types of systems were used: a palladium (II) complex formed in situ; and one prepared prior to the catalytic reaction. In general, the palladium complexes studied achieved high conversions in an average reaction time of less than 2 hr, which is less than that for the standard system (Pd (II)/PPh₃) used. The pre‐synthesized complexes were faster than their in situ counterparts, as the latter require an induction time to form the Pd/P^N species. The structure and electronic properties of the ligand P^N can influence both the activity and the selectivity of the reaction, stabilizing the acyl‐palladium intermediates formed in a better manner.     

Oxidation kinetics of thin copper films and wetting behaviour of copper and Organic Solderability Preservatives (OSP) with lead-free solder

The oxide formation on thin copper films deposited on Si wafer was studied by XPS, SEM and Sequential Electrochemical Reduction Analysis SERA. The surfaces were oxidized in air with a reflow oven as used in electronic assembly at temperatures of 100 °C, 155 °C, 200 °C, 230 °C and 260 °C. The SERA analyses detected only the formation of Cu₂O but the XPS analysis done for the calibration of the SERA equipment proved also the presence of a CuO layer smaller than 2 nm above the Cu₂O oxide. The oxide growth follows a power-law dependence on time within this temperature range and an activation energy of 33.1 kJ/mol was obtained. The wettability of these surfaces was also determined by measuring the contact angle between solder and copper substrate after the soldering process. A correlation between oxide thickness and wetting angle was established. It was found that the wetting is acceptable only when the oxide thickness is smaller than 16 nm. An activation energy of 27 kJ/mol was acquired for the spreading of lead free solder on oxidized copper surfaces.From wetting tests on copper surfaces protected by Organic Solderability Preservatives (OSP), it was possible to calculate the activation energy for the thermal decomposition of these protective layers.     

High-fidelity front-end for high-power, high temporal quality few-cycle lasers

A 80???J, 6?fs, CEP-stable high-contrast injector is demonstrated. The device relies on standard pulse post-compression in hollow-core fiber followed by a temporal filter based on cross-polarized wave generation. Pulses with a Gaussian spectrum over 350?nm, centered at 750?nm, are generated. Temporal measurements show that the contrast of the few-cycle pulses is enhanced on a femtosecond and picosecond time scale. The carrier-envelope phase stability is preserved (0.3?rad RMS). These performances make the system an ideal seed laser for high-power, high-contrast OPCPA systems.     

A high statistics measurement of the Lambda(+)(c) lifetime

A high statistics measurement of the Lambda(+)(c) lifetime from the Fermilab fixed-target FOCUS photoproduction experiment is presented. We describe the analysis technique with particular attention to the determination of the systematic uncertainty. The measured value of 204.6 +/- 3.4 (stat) +/- 2.5 (syst) fs from 8034 +/- 122 Lambda(+)(c)-->pK(-)pi(+) decays represents a significant improvement over the present world average.     

Strongly enhanced hole-phonon coupling in the metallic state of the dilute two-dimensional hole gas

We have studied the temperature dependent phonon emission rate P(T) of a strongly interacting (r(s) > or =22) dilute 2D GaAs hole system using a standard carrier heating technique. In the still poorly understood metallic state, we observe that P(T) changes from P(T) approximately T5 to P(T) approximately T7 above 100 mK, indicating a crossover from screened piezoelectric (PZ) coupling to screened deformation potential (DP) coupling for hole-phonon scattering. Quantitative comparison with theory shows that the long range PZ coupling between holes and phonons has the expected magnitude; however, in the metallic state, the short range DP coupling between holes and phonons is almost 20 times stronger than expected from theory. The density dependence of P(T) shows that it is easier to cool low-density 2D holes in GaAs than higher density 2D hole systems.