On the Synthesis of Pyrrolobenzo[<Emphasis Type="Italic">b</Emphasis>]thieno[1,4]diazepines

Summary. 2-Amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carbonitrile was converted into the corresponding 2-(pyrrol-1-yl) derivative, followed by reduction of the latter compound into the corresponding amine. This amine and its acyl, aroyl, and arylidene derivatives were used as synthons in the synthesis of several title compounds.     

Multinuclear NMR study of the structure and micro-dynamics of counterions and water molecules within clay colloids

Multinuclear NMR spectroscopy, relaxation and diffusion measurements were used recently to extract dynamical information on the long-time mobility of the water molecules and the neutralizing counterions condensed within the electrostatic well in the vicinity of the basal surface of clay particles. Multi-scale numerical modeling was used to interpret the NMR relaxation measurements and illustrate the interdependency between the solvent and ionic mobility and the organization of the anisotropic clay particles within the colloidal dispersions.     

Investigation on laser brazing AA6056 Al alloy to XC18 low-carbon steel

Based on the studies of influence of YAG laser heating conditions for Al alloy melt and steel on wettability,the mechanics of the laser overlap braze welding of 6056 Al and XC18 steel sheet has been investigated.Under the temperature range which is above the melting point of the Al alloy and below the melting point of the steel, two dissimilar metals can be joined by means of laser braze welding. There is no crack observed in the joining area, i.e. Al-Fe intermetallic phase (Fe3Al/FeAl/FeAl3/Fe2Al5) layer formed by solution and diffusion between liquid-solid interface. The temperature range can be defined as the process temperatures of laser braze welding of Al-Fe materials. Selecting a higher laser heating temperature can improve the wettability of Al melt to steel surface, but the intermetallic phase layer is also thicker. When the laser heating temperature is so high that the joining surface of steel is melted, there is a crack trend in the joining area.     

Squeeze flow of Bingham fluids under slip with friction boundary condition

This paper develops a theoretical analysis of a Bingham fluid in slipping squeeze flow. The flow field decomposition consists in combining a central extensional flow zone in the plane of symmetry and shear flow zones near the plates. It is also considered that the slipping zone is located around a central sticking zone as previously shown from experiments. It is assumed that the shear stress at the plates is constant in the slipping zone and equals a fixed friction yield value. The squeeze force required to compress a Bingham fluid under the slipping behaviour as well as the radial evolution of the transition point between both sticking and slipping zones are finally determined.     

Capillary electrophoresis for rapid identification of monoclonal antibodies for routine application in hospital

mAbs are widely used in cancer therapy. Their compounding, performed just before their administration to patients, is executed in a production unit of the hospital. Identification of these drugs, individually prepared in bags for infusion before patient administration, is of paramount importance to detect potential mistakes during compounding stage. A fast and reliable analytical method based on CZE combined to a cationic capillary coating (hexadimethrine bromide) was developed for identification of the most widely used compounded therapeutic for cancer therapy (bevacizumab, cetuximab, rituximab, and trastuzumab). Considering the high structural and physico‐chemical similarities of these mAbs, an extensive optimization of the BGE composition has been performed. The addition of perchlorate ions and polysorbate in the BGE greatly increased the resolution. To validate the method, an internal standard was used and the relative migration times (RTm) were estimated. Very satisfactory RSDs of the RTm for rituximab (0.76%), cetuximab (0.46%), bevacizumab (0.31%), and trastuzumab (0.60%) were obtained. The intraday and interday RSD of the method were less than 0.32 and 1.3%, respectively for RTm. Significant differences between theses RTms have been demonstrated allowing mAbs identification. Finally, accurate mAbs identification has been demonstrated by a blind test.     

Slipping zone location in squeeze flow

In squeeze flow rheometry, the main problem is the boundary condition between the squeezed material and the plates. Therefore, the crucial assumption is to know the location and the shape of the sample part where wall slip may or may not occur. This question is investigated from experimental results. For this, squeeze flow experiments are carried out to visualize the flow pattern at the walls. Influence of boundary conditions is particularly studied using different plate surface condition. As a result, with wall slipping conditions, we propose a flow modelling divided into two zones: a circular central zone of the sample sticks on the plates and, beyond that zone, the sample slips at the plates with friction.     

Understanding and improving direct UV detection of monosaccharides and disaccharides in free solution capillary electrophoresis

Direct UV detection of carbohydrates in free solution capillary electrophoresis at 270 nm is made possible by a photo-oxidation reaction. Glucose, rhamnose and xylose were shown to have unique UV absorption spectra hypothesizing different UV absorbing intermediates for their respective photo-oxidation. NMR spectroscopy of the photo-oxidation end products proved they consisted of carboxylates and not malondialdehyde as previously theorized and that oxygen thus plays a key role in the photo-oxidation pathway. Adding the photo-initiator Irgacure^® 2959 in the background electrolyte increased sensitivity by 40% at an optimum concentration of 1 × 10⁻⁴ mM and 1 × 10⁻⁸ mM for conventional 50 μm i.d. capillaries and for the corresponding extended light path capillaries, respectively.